2-(Methylamino)ethanol → 2-(Methyl(2-hydroxyethyl)amino)benzothiazole

HRID 263980

反応式

HRID 263980 の反応式
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

反応物 2

HCID 80162-(Methylamino)ethanolHCID 119872-Chlorobenzothiazole

生成物 1

HCID 6008992-(Methyl(2-hydroxyethyl)amino)benzothiazole

試薬・触媒・溶媒 1

HCID 962Water溶媒

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.

後処理

  1. temperatureAfter cooling
  2. extractionextracted with dichloromethane (2×100 ml)
  3. dry with materialthe organic extracts were dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-5befa6cd162645a5a0dd0b7ac3c26f2d
出典データセット
uspto-grants-1997_07
特許番号
US05646169

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