Acetic Acid → 1-Methyl-1,5-dihydro-imidazo[4,5-c]pyridine-4-thione
反応式
Cl[C:2]1[C:7]2[N:8]=[CH:9][N:10]([CH3:11])[C:6]=2[CH:5]=[CH:4][N:3]=1.O.[SH2:13].[Na].O.C(O)(=O)C>CN(C)C=O>[CH3:11][N:10]1[C:6]2[CH:5]=[CH:4][NH:3][C:2](=[S:13])[C:7]=2[N:8]=[CH:9]1参加物
6
反応条件
- 温度
- 5 °C
実験手順
4.00 g (23.9 mmol) of 4-chloro-1-methyl-1H-imidazo[4,5-c]pyridine in 27 ml of dimethylformamide were stirred at 115° C. for 18 hours with 8.10 g (95.6 mmol) of sodium hydrogen sulphide hydrate. After cooling the mixture was treated with 110 ml of water, adjusted to pH 4 with acetic acid and stirred at 5° C. while cooling with ice for 15 min. The precipitate was filtered off and washed with water. After drying there were obtained 3.73 g (95%) of 1-methyl-1,5-dihydro-imidazo[4,5-c]pyridine-4-thione as white crystals with m.p. >300° C.
後処理
- temperatureAfter cooling the mixture
- temperaturewhile cooling with ice for 15 min
- filtrationThe precipitate was filtered off
- washwashed with water
- customAfter drying there
出典と根拠
- ORDレコード
- ord-505a70ca758b4c6cae28240203f97f47
- 出典データセット
- uspto-grants-1999_02
- 特許番号
- US05869500
反応ノート
読み込み中…