Sodium Hydroxide → 4-(2-chlorophenyl)-2-[5-(trifluoromethyl)-2H-tetrazol-2-yl]methylpyrimidine-5-carboxylic acid

HRID 1958086노트

반응식

HRID 1958086 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:13]([C:14]([O:16]CC)=[O:15])=[CH:12][N:11]=[C:10]([CH2:19][N:20]2[N:24]=[N:23][C:22]([C:25]([F:28])([F:27])[F:26])=[N:21]2)[N:9]=1.[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:13]([C:14]([OH:16])=[O:15])=[CH:12][N:11]=[C:10]([CH2:19][N:20]2[N:24]=[N:23][C:22]([C:25]([F:26])([F:27])[F:28])=[N:21]2)[N:9]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 67125210ethyl 4-(2-chlorophenyl)-2-[5-(trifluoromethyl)-2H-tetrazol-2-yl]methylpyrimidine-5-carboxylate

생성물 1

HCID 671252154-(2-chlorophenyl)-2-[5-(trifluoromethyl)-2H-tetrazol-2-yl]methylpyrimidine-5-carboxylic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

An amount of 1.74 g (4.21 mmol) of ethyl 4-(2-chlorophenyl)-2-{[5-(trifluoromethyl)-2H-tetrazol-2-yl]methyl}pyrimidine-5-carboxylate was dissolved in 12 ml of ethanol and the solution was admixed dropwise at 0° C. with 45% strength aqueous sodium hydroxide solution (5.05 mmol). The reaction was stirred for a further hour and warmed to RT. The ethanol was then removed under reduced pressure and the residue was admixed with ice-water (10 ml). The aqueous phase was extracted with ethyl acetate. The organic phase was discarded. Then the aqueous phase was adjusted to a pH of 3 using hydrochloric acid, and again extracted with ethyl acetate (3×20 ml). The combined organic phases were dried over sodium sulphate.

후처리

  1. customThe ethanol was then removed under reduced pressure
  2. extractionThe aqueous phase was extracted with ethyl acetate
  3. extractionagain extracted with ethyl acetate (3×20 ml)
  4. dry with materialThe combined organic phases were dried over sodium sulphate

출처 및 근거

ORD 기록
ord-55ab3ccd554846b2b458bbf2e1a1472c
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410106B2

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