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Triethylamine → HCID 57687747, 화합물

HRID 1880817
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HRID 1880817 반응식
[C:1]([O:5][C:6](=[O:20])[NH:7][CH2:8][CH2:9][CH2:10][CH2:11][C@H:12]([NH:15][CH2:16][CH:17]([CH3:19])[CH3:18])[CH2:13][OH:14])([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:28]([C:30]1[CH:35]=[CH:34][C:33]([S:36](Cl)(=[O:38])=[O:37])=[CH:32][CH:31]=1)#[N:29].C([O-])(O)=O.[Na+]>C(Cl)Cl>[C:1]([O:5][C:6](=[O:20])[NH:7][CH2:8][CH2:9][CH2:10][CH2:11][C@H:12]([N:15]([S:36]([C:33]1[CH:32]=[CH:31][C:30]([C:28]#[N:29])=[CH:35][CH:34]=1)(=[O:38])=[O:37])[CH2:16][CH:17]([CH3:18])[CH3:19])[CH2:13][OH:14])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 394974-Cyanobenzenesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 57687748HCID 57687748, 화합물

생성물 1

HCID 57687747HCID 57687747, 화합물수율 36%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

(S)-(6-Hydroxy-5-isobutylamino-hexyl)-carbamic acid tert-butyl ester (4) (1.85 g) was dissolved in 50 mL CH2Cl2. Triethylamine (1.05 eq) and 4-cyano benzene sulfonylchloride (1 eq) were added and the mixture was stirred overnight. Saturated NaHCO3 (50 mL) was added, the mixture was well shaken. Organic layer was separated, dried on MgSO4, filtrated and evaporated. The crude compound was purified by column chromatography using EtOAc-heptane (1-3) as the eluent. Fractions containing the product were evaporated yielding (1.06 g, 36%) of a solid.

후처리

  1. stirringthe mixture was well shaken
  2. customOrganic layer was separated
  3. customdried on MgSO4
  4. filtrationfiltrated
  5. customevaporated
  6. customThe crude compound was purified by column chromatography
  7. additionFractions containing the product
  8. customwere evaporated

출처 및 근거

ORD 기록
ord-cfed406870aa4d9ea3762938a64db134
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318779B2

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