Sodium Hydroxide → HCID 67288943, 화합물

HRID 1626503노트

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HRID 1626503 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][C:13]1[CH:18]=[CH:17][C:16]([C:19](=[O:34])[NH:20][C:21]3[CH:25]=[CH:24][N:23]([C:26]4[CH:31]=[CH:30][C:29]([F:32])=[C:28]([F:33])[CH:27]=4)[N:22]=3)=[CH:15][CH:14]=1)[O:8][CH2:7][CH2:6][CH:5]2[C:35]([O:37]CC)=[O:36].[OH-].[Na+]>C1COCC1.CO>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][C:13]1[CH:18]=[CH:17][C:16]([C:19](=[O:34])[NH:20][C:21]3[CH:25]=[CH:24][N:23]([C:26]4[CH:31]=[CH:30][C:29]([F:32])=[C:28]([F:33])[CH:27]=4)[N:22]=3)=[CH:15][CH:14]=1)[O:8][CH2:7][CH2:6][CH:5]2[C:35]([OH:37])=[O:36]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 67288081HCID 67288081, 화합물

생성물 1

HCID 67288943HCID 67288943, 화합물수율 61.3%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

실험 절차

To a solution of ethyl 6-chloro-7-(4-(1-(3,4-difluorophenyl)-1H-pyrazol-3-ylcarbamoyl)phenoxy)chroman-4-carboxylate (0.067 g, 0.121 mmol) in 3:1 THF/MeOH (1 ml) was added 1M sodium hydroxide (0.133 ml, 0.133 mmol), and the reaction was allowed to stir for 16 hours. The reaction was concentrated, acidified with dilute HCl, and extracted twice with EtOAc. The combined organics were dried over anhydrous sodium sulfate, filtered, and concentrated to yield the desired product (0.039 g, 0.0742 mmol, 61.3% yield). MS (apci): m/z=526.1 (M+H).

후처리

  1. concentrationThe reaction was concentrated
  2. extractionextracted twice with EtOAc
  3. dry with materialThe combined organics were dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-6aa34381d2e0445c9a91f498e84a36c0
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785445B2

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