反応式
Cl[C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[CH3:11][NH:12][CH2:13][CH2:14][OH:15]>O>[CH3:11][N:12]([CH2:13][CH2:14][OH:15])[C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1参加物
4
反応条件
- 温度
- 120 °C
実験手順
A mixture of 2-chlorobenzothiazole (8.5 g) and 2-methylaminoethanol (20 ml) was heated at 120° C. under pressure in a sealed, glass lined, stainless steel reaction vessel for 18 hours. After cooling, the oil was added to water (100 ml), extracted with dichloromethane (2×100 ml), the organic extracts were dried (MgSO4), filtered and evaporated to dryness Chromatography of the residual oil on silica-gel in 21/2% methanol in dichloromethane gave the title compound which was used in Preparation 1 without further purification. 1H NMR δ (CDCl3) 3.15 (3H, s); 3.4-4.0 (4H, m); 4.7 (1H, broad s, exchanges with D2O; 6.8-7.6 (4H, complex).
後処理
- temperatureAfter cooling
- extractionextracted with dichloromethane (2×100 ml)
- dry with materialthe organic extracts were dried (MgSO4)
- filtrationfiltered
- customevaporated to dryness Chromatography of the residual oil on silica-gel in 21/2% methanol in dichloromethane
出典と根拠
- ORDレコード
- ord-e4a9744186e84353b208b1e4f1e9881e
- 出典データセット
- uspto-grants-1991_03
- 特許番号
- US05002953
関連ノート
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