Hydrochloric Acid → HCID 19600266, 화합물

HRID 611256노트

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HRID 611256 반응식
[C:1]([C:9]1[CH:29]=[CH:28][C:12]([C:13]([N:15]2[CH2:20][CH2:19][C:18]3[CH:21]=[C:22]([C:24]([O:26]C)=[O:25])[O:23][C:17]=3[CH2:16]2)=[O:14])=[CH:11][CH:10]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>O1CCCC1.[OH-].[Na+]>[C:1]([C:9]1[CH:10]=[CH:11][C:12]([C:13]([N:15]2[CH2:20][CH2:19][C:18]3[CH:21]=[C:22]([C:24]([OH:26])=[O:25])[O:23][C:17]=3[CH2:16]2)=[O:14])=[CH:28][CH:29]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

실험 절차

To a solution of 126 mg (0.324 mmol) of methyl 6-(4-benzoylbenzoyl)-4,5,6,7-tetrahydrofuro[2,3-c]pyridine-2-carboxylate in 10 ml of tetrahydrofuran, 1 ml of 2 N aqueous sodium hydroxide was added, followed by stirring at room temperature for 1 day. The reaction mixture was acidified with 10 ml of 1 N hydrochloric acid and extracted with diethyl ether 3 times. The combined organic layer was dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (ethyl acetate/methanol=4/1 to chloroform/methanol=1/1) to yield the desired product.

후처리

  1. extractionextracted with diethyl ether 3 times
  2. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe resulting crude product was purified by silica gel column chromatography (ethyl acetate/methanol=4/1 to chloroform/methanol=1/1)

출처 및 근거

ORD 기록
ord-3d4203d0a7e94fc0b05be808b7d77e36
출처 데이터셋
uspto-grants-1999_12
특허 번호
US05998433

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