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Hydrochloric Acid → HCID 86721282, 화합물

HRID 1750440
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HRID 1750440 반응식
[C:1]([N:5]1[C:9]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)=[C:8]([C:18]2[S:19][CH:20]=[C:21](/[CH:23]=[CH:24]/[C:25]([O:27]CC)=[O:26])[N:22]=2)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+].Cl>C1COCC1.CO>[C:1]([N:5]1[C:9]([C:10]2[CH:11]=[CH:12][C:13]([O:16][CH3:17])=[CH:14][CH:15]=2)=[C:8]([C:18]2[S:19][CH:20]=[C:21](/[CH:23]=[CH:24]/[C:25]([OH:27])=[O:26])[N:22]=2)[CH:7]=[N:6]1)([CH3:4])([CH3:2])[CH3:3]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86721281HCID 86721281, 화합물

생성물 1

HCID 86721282HCID 86721282, 화합물수율 97%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

To a mixed solution of the compound (200 mg, 0.49 mmol) obtained in step 4 in THF (2 mL) and methanol (2 mL) was added 1N aqueous sodium hydroxide solution (0.972 ml, 0.97 mmol) at room temperature, and the mixture was stirred at 60° C. for 3 hr. The reaction mixture was cooled to room temperature, and 1N hydrochloric acid was added until the mixture became pH 2-3. The mixture was extracted with ethyl acetate, the organic layer was dried, and the solvent was evaporated under reduced pressure to give (E)-3-(2-(1-(tert-butyl)-5-(4-methoxyphenyl)-1H-pyrazol-4-yl)thiazol-4-yl)acrylic acid (180.7 mg, 0.471 mmol, 97%) as a white powder.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionThe mixture was extracted with ethyl acetate
  3. customthe organic layer was dried
  4. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-97437364c72e4918b7c7bd3e263b2d98
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09156837B2

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