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

HRID 1374928노트

반응식

HRID 1374928 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

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온도
135 °C

실험 절차

The neat mixture of R (+) 2-chloro-1-phenylethanol (4.32 g., 27.6 mmol) and 4,5-dimethylthiazole (3.12 g, 27.6 mmol) were heated with stirring at 135° C. for 25 hrs. It was cooled to room temperature and water (30 mL) was added to the reaction mixture with stirring. The solution was extracted with ether (30 mL). The ether extract was again extracted with water (30 mL). The combined water layer was evaporated to dryness and the residue was crystallized with a mixture of acetonitrile and methyl tert-butyl ether. Yield: 0.44 g. (5.4%); mp. 187–189° C.; [α]D25+52.009 (Water, c=1.7824).

후처리

  1. temperaturewere heated
  2. temperatureIt was cooled to room temperature
  3. stirringwith stirring
  4. extractionThe solution was extracted with ether (30 mL)
  5. extractionThe ether extract
  6. extractionwas again extracted with water (30 mL)
  7. customThe combined water layer was evaporated to dryness
  8. customthe residue was crystallized with a mixture of acetonitrile and methyl tert-butyl ether

출처 및 근거

ORD 기록
ord-b303480c87344e63b1bfb1137df6da67
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07166625B2

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