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Water → HCID 22932162, 화합물

HRID 1351089
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HRID 1351089 반응식
[OH:1][CH2:2][CH2:3][NH:4][NH2:5].[CH3:6][CH:7]([CH3:21])[C:8](=O)[CH2:9][C:10]([O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=S.C(N(CC)CC)C.O>C(#N)C>[CH2:13]([O:12][C:10]1[CH:9]=[C:8]([CH:7]([CH3:21])[CH3:6])[N:4]([CH2:3][CH2:2][OH:1])[N:5]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 80172-HydrazinoethanolHCID 8471TriethylamineHCID 22932184HCID 22932184, 화합물

생성물 1

HCID 22932162HCID 22932162, 화합물수율 90.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

2-Hydroxyethylhydrazine (1.90 g) was added to a solution of O-Benzyl 4-methyl-3-oxothiopentanoate (5.90 g) and triethylamine (5.05 g) in acetonitrile (60 mL), and the mixture was stirred at room temperature for 3 hours. The reaction mixture was poured into water, and the mixture was extracted with diethyl ether. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: hexane/ethyl acetate=1/1) to give the title compound (5.90 g).

후처리

  1. extractionthe mixture was extracted with diethyl ether
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel (eluent: hexane/ethyl acetate=1/1)

출처 및 근거

ORD 기록
ord-c00c74838268406e860fe4bd3e52d014
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07217697B2

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