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Ethyl Acetate → HCID 21939926, 화합물

HRID 1242915
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HRID 1242915 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([C:14]([NH:16][C:17]3[CH:37]=[CH:36][C:20]([C:21]([CH:23]4[CH2:28][CH2:27][CH2:26][N:25]([C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30])[CH2:24]4)=[O:22])=[CH:19][CH:18]=3)=[O:15])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[BH4-].[Na+].C(OCC)(=O)C>CO.O1CCCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[CH:10][C:11]([C:14]([NH:16][C:17]3[CH:37]=[CH:36][C:20]([CH:21]([OH:22])[CH:23]4[CH2:28][CH2:27][CH2:26][N:25]([C:29]([O:31][C:32]([CH3:34])([CH3:33])[CH3:35])=[O:30])[CH2:24]4)=[CH:19][CH:18]=3)=[O:15])=[CH:12][CH:13]=2)=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8857Ethyl AcetateHCID 4311764Sodium borohydrideHCID 21939751HCID 21939751, 화합물

생성물 1

HCID 21939926HCID 21939926, 화합물수율 96.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

tert-Butyl 3-[4-[[(4′-chloro[1,1′-biphenyl]-4-yl)carbonyl]amino]benzoyl]-1-piperidinecarboxylate (506 mg, 0.975 mmol) obtained in Example 127-1) was dissolved in a mixed solution of methanol and tetrahydrofuran (1:1) (10 ml). Sodium borohydride (73.8 mg, 1.95 mmol) was added to the solution under ice-cooling, which was stirred at room temperature for 1 hour. Ethyl acetate was added to the reaction mixture, which was washed with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and then the solvent was distilled out under reduced pressure. Diisopropyl ether was added to the residue, to give the titled compound (488 mg) as a colorless powder.

후처리

  1. temperaturecooling
  2. washwas washed with saturated aqueous sodium chloride solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled out under reduced pressure
  5. additionDiisopropyl ether was added to the residue

출처 및 근거

ORD 기록
ord-b375baacac6c41af867bd09f940bfbed
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07115750B1

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