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Sodium Hydroxide → HCID 59516080, 화합물

HRID 1160561
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HRID 1160561 반응식
[OH-].[Na+].[C:3]([C:7]1[N:11]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([C:19]([F:22])([F:21])[F:20])[CH:13]=2)[N:10]=[CH:9][C:8]=1[C:23]([O:25]CC)=[O:24])([CH3:6])([CH3:5])[CH3:4]>CO>[C:3]([C:7]1[N:11]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([C:19]([F:20])([F:22])[F:21])[CH:13]=2)[N:10]=[CH:9][C:8]=1[C:23]([OH:25])=[O:24])([CH3:6])([CH3:4])[CH3:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 59516093HCID 59516093, 화합물

생성물 1

HCID 59516080HCID 59516080, 화합물수율 83%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
80 °C

실험 절차

A solution of Sodium hydroxide (6.67 mL, 13.34 mmol) was added in one portion to a stirred solution of ethyl 5-tert-butyl-1-(4-chloro-3-(trifluoromethyl)phenyl)-1H-pyrazole-4-carboxylate (Intermediate#120) (1 g, 2.67 mmol) in methanol (20 mL). The resulting suspension was stirred at 80° C. for 6 hours. The resulting mixture was evaporated to remove the methanol, washed with ether (20 mL). The reaction mixture was acidified with 2M HCl, extracted with ethyl acetate(2×30 mL) The organic layers were combined and washed with water (10 mL) and brine (10 mL), dried over MgSO4, filtered and evaporated to afford pure 5-tert-butyl-1-(4-chloro-3-(trifluoromethyl)phenyl)-1H-pyrazole-4-carboxylic acid (0.766 g, 83%).

후처리

  1. customThe resulting mixture was evaporated
  2. customto remove the methanol
  3. washwashed with ether (20 mL)
  4. extractionextracted with ethyl acetate(2×30 mL) The organic layers
  5. washwashed with water (10 mL) and brine (10 mL)
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-4aae567bf84140728baa628f2002937c
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07816391B2

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