Hydrochloric Acid → HCID 86642839, 화합물

HRID 1667770노트

반응식

HRID 1667770 반응식
C([Si]([O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:18]=[C:17](F)[C:16]([N+:20]([O-:22])=[O:21])=[CH:15][C:14]=1[O:23][CH3:24])(C)C)(C)(C)C.[NH2:25][C:26]1[S:27][C:28]([C:38]([NH2:40])=[O:39])=[C:29]([C:31]2[CH:36]=[CH:35][CH:34]=[C:33]([Cl:37])[CH:32]=2)[N:30]=1.C(=O)([O-])[O-].[Cs+].[Cs+].Cl>O.CN(C)C=O>[Cl:37][C:33]1[CH:32]=[C:31]([C:29]2[N:30]=[C:26]([NH:25][C:17]3[CH:18]=[C:13]([O:12][CH2:11][CH2:10][CH2:9][OH:8])[C:14]([O:23][CH3:24])=[CH:15][C:16]=3[N+:20]([O-:22])=[O:21])[S:27][C:28]=2[C:38]([NH2:40])=[O:39])[CH:36]=[CH:35][CH:34]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 10796Cesium carbonateHCID 166588232-Amino-4-(3-chlorophenyl)thiazole-5-carboxamideHCID 67428158Tert-butyl-[3-(5-fluoro-2-methoxy-4-nitro-phenoxy)-propoxy]-dimethyl-silane

생성물 1

HCID 86642839HCID 86642839, 화합물수율 85.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 0.469 g (1.31 mmole) of tert-butyl-[3-(5-fluoro-2-methoxy-4-nitro-phenoxy)-propoxy]-dimethyl-silane (IV.42), 0.331 g (1.31 mmole) of 2-amino-4-(3-chloro-phenyl)-thiazole-5-carboxylic acid amide (V.2), 1.28 g (3.93 mmole) of cesium carbonate and 5 mL of dimethylformamide was heated at 70 degrees for 3 hours. The mixture was cooled and 3 mL of 6M hydrochloric acid was added dropwise. Stirring was continued for 15 minutes. The mixture was poured into 50 mL of water, and the precipitated orange solid was collected by filtration, washed with water, and air-dried to give 0.535 g of 4-(3-chloro-phenyl)-2-[5-(3-hydroxy-propoxy)-4-methoxy-2-nitro-phenylamino]-thiazole-5-carboxylic acid amide (VI.42).

후처리

  1. temperaturewas heated at 70 degrees for 3 hours
  2. temperatureThe mixture was cooled
  3. filtrationthe precipitated orange solid was collected by filtration
  4. washwashed with water
  5. customair-dried

출처 및 근거

ORD 기록
ord-3aba5318ed1049ba9a0c45ee6f9510aa
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08044213B2

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