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

HRID 2113422노트

반응식

HRID 2113422 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
135 °C

실험 절차

The neat mixture of 2-chloro-1-phenylethanol (2.34 g, 14.9 mmol) and 4,5-dimethylthiazole (1.69 g, 14.9 mmol) 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.

후처리

  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

출처 및 근거

ORD 기록
ord-6f919ce58c7341598185eaf429a5b63f
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07432254B2

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