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Triethylamine → Methanesulfonic acid 5-(3-chloro-4-cyano-phenoxymethyl)-2-(4-trifluoromethyl-phenyl)-thiazol-4-ylmethyl ester

HRID 2233592
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HRID 2233592 반응식
[Cl:1][C:2]1[CH:9]=[C:8]([O:10][CH2:11][C:12]2[S:16][C:15]([C:17]3[CH:22]=[CH:21][C:20]([C:23]([F:26])([F:25])[F:24])=[CH:19][CH:18]=3)=[N:14][C:13]=2[CH2:27][OH:28])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[CH3:29][S:30](Cl)(=[O:32])=[O:31].C(N(CC)CC)C>ClCCl>[Cl:1][C:2]1[CH:9]=[C:8]([CH:7]=[CH:6][C:3]=1[C:4]#[N:5])[O:10][CH2:11][C:12]1[S:16][C:15]([C:17]2[CH:22]=[CH:21][C:20]([C:23]([F:25])([F:24])[F:26])=[CH:19][CH:18]=2)=[N:14][C:13]=1[CH2:27][O:28][S:30]([CH3:29])(=[O:32])=[O:31]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 592961782-Chloro-4-[4-hydroxymethyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-ylmethoxy]-benzonitrile

생성물 1

HCID 59296164Methanesulfonic acid 5-(3-chloro-4-cyano-phenoxymethyl)-2-(4-trifluoromethyl-phenyl)-thiazol-4-ylmethyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

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온도
0 °C

실험 절차

1.8 g 2-Chloro-4-[4-hydroxymethyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-ylmethoxy]-benzonitrile were suspended in 50 ml dichloromethane and cooled in an ice bath. 0.39 ml methanesulfonylchloride and 0.89 ml triethylamine were added. The resulting mixture was stirred at 0° C. for one hour then washed with water and brine, dried over MgSO4. The solvent was removed in vacuo to obtain 1.0 g methanesulfonic acid 5-(3-chloro-4-cyano-phenoxymethyl)-2-(4-trifluoromethyl-phenyl)-thiazol-4-ylmethyl ester as pale yellow solid.

후처리

  1. temperaturecooled in an ice bath
  2. washthen washed with water and brine
  3. dry with materialdried over MgSO4
  4. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-93fdfd7424f44c0b935b3a1c79aba53f
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07709509B2

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