4,5-Dimethylthiazole → Thiazolium, 3-(2-hydroxy-2-phenylethyl)-4,5-dimethyl-, chloride

HRID 989912ノート

反応式

HRID 989912 の反応式
[Cl:1][CH2:2][CH:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[OH:4].[CH3:11][C:12]1[N:13]=[CH:14][S:15][C:16]=1[CH3:17]>O>[Cl-:1].[C:5]1([CH:3]([OH:4])[CH2:2][N+:13]2[C:12]([CH3:11])=[C:16]([CH3:17])[S:15][CH:14]=2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

4

反応物 2

HCID 625104,5-DimethylthiazoleHCID 928982-Chloro-1-phenylethanol

生成物 1

HCID 9838299Thiazolium, 3-(2-hydroxy-2-phenylethyl)-4,5-dimethyl-, chloride

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
135 °C

実験手順

The neat mixture of 2-chloro-l-phenylethanol (2.34 g, 14.9 mmole) and 4,5-dimethylthiazole (1.69 g, 14.9 mmole) were heated with stirring at 135° C. for 28 hrs. It was cooled to room temperature and water (30 mL) was added to the reaction mixture with stirring, and then was extracted with ether (30 mL). The water layer was treated with actived carbon and evaporated to dryness. It was crystallized from a mixture of acetonitrile and ether to give a racemic product as prisms; 0.39 g (9.7%); mp. 201-203° C.

後処理

  1. temperaturewere heated
  2. temperatureIt was cooled to room temperature
  3. stirringwith stirring
  4. extractionwas extracted with ether (30 mL)
  5. additionThe water layer was treated with actived carbon
  6. customevaporated to dryness
  7. customIt was crystallized from a mixture of acetonitrile and ether

出典と根拠

ORDレコード
ord-6bfc94e3239146c2931353c484c5939a
出典データセット
uspto-grants-2002_10
特許番号
US06458819B1

反応ノート

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