lithium iodide in N,N,N',N',N'',N''-hexamethylphosphoric triamide 20 h; Heating;

1: 1.) Br2, 2.) H2O / 1.) CCl4, reflux, 5 min, irradiation, 2.) dioxan, reflux, 4 h 2: 240 mg / BCl3 / CH2Cl2 / 4.5 h / Ambient temperature 3: toluene-p-sulphonic acid monohydrate / dimethylformamide / 82 h 4: 146 mg / pyridinium chlorochromate, sodium acetate / CH2Cl2 / 4 h 5: 59 mg / acetic acid (aq) / 24 h / Heating 6: 6.5 mg / LiI / hexamethylphosphoric acid triamide / 20 h / Heating View Scheme

1: K2CO3 / dimethylformamide 2: 1.) Br2, 2.) H2O / 1.) CCl4, reflux, 5 min, irradiation, 2.) dioxan, reflux, 4 h 3: 240 mg / BCl3 / CH2Cl2 / 4.5 h / Ambient temperature 4: toluene-p-sulphonic acid monohydrate / dimethylformamide / 82 h 5: 146 mg / pyridinium chlorochromate, sodium acetate / CH2Cl2 / 4 h 6: 59 mg / acetic acid (aq) / 24 h / Heating 7: 6.5 mg / LiI / hexamethylphosphoric acid triamide / 20 h / Heating View Scheme

1: 240 mg / BCl3 / CH2Cl2 / 4.5 h / Ambient temperature 2: toluene-p-sulphonic acid monohydrate / dimethylformamide / 82 h 3: 146 mg / pyridinium chlorochromate, sodium acetate / CH2Cl2 / 4 h 4: 59 mg / acetic acid (aq) / 24 h / Heating 5: 6.5 mg / LiI / hexamethylphosphoric acid triamide / 20 h / Heating View Scheme

1: 59 mg / acetic acid (aq) / 24 h / Heating 2: 6.5 mg / LiI / hexamethylphosphoric acid triamide / 20 h / Heating View Scheme

1: 146 mg / pyridinium chlorochromate, sodium acetate / CH2Cl2 / 4 h 2: 59 mg / acetic acid (aq) / 24 h / Heating 3: 6.5 mg / LiI / hexamethylphosphoric acid triamide / 20 h / Heating View Scheme

1: toluene-p-sulphonic acid monohydrate / dimethylformamide / 82 h 2: 146 mg / pyridinium chlorochromate, sodium acetate / CH2Cl2 / 4 h 3: 59 mg / acetic acid (aq) / 24 h / Heating 4: 6.5 mg / LiI / hexamethylphosphoric acid triamide / 20 h / Heating View Scheme

alkali durch hydrolytische Spaltung;

1: 96 percent / 1,2-dimethoxy-ethane / 2 h / Heating 2: 74 percent / hydrogen / 10percent palladium on carbon / various solvent(s) / 2 h / 140 °C View Scheme

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