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Triethylamine → HCID 76488224, 화합물

HRID 1599713
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HRID 1599713 반응식
[Br:1][CH2:2][CH2:3][CH2:4][S:5](Cl)(=[O:7])=[O:6].NCCCCS([NH:17][CH2:18][CH:19]1[CH2:23][CH2:22][CH2:21][N:20]1[C:24](=[O:41])[CH:25]([NH:33][C:34](=[O:40])[O:35][C:36]([CH3:39])([CH3:38])[CH3:37])[CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)(=O)=O.C(N(CC)CC)C>ClCCl>[Br:1][CH2:2][CH2:3][CH2:4][S:5]([NH:17][CH2:18][CH:19]1[CH2:23][CH2:22][CH2:21][N:20]1[C:24](=[O:41])[CH:25]([NH:33][C:34](=[O:40])[O:35][C:36]([CH3:37])([CH3:39])[CH3:38])[CH2:26][C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)(=[O:7])=[O:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 2893293-Bromopropane-1-sulfonyl chlorideHCID 67846374HCID 67846374, 화합물

생성물 1

HCID 76488224HCID 76488224, 화합물수율 72%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

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온도
-10 °C

실험 절차

A solution of Part A 3-bromopropyl sulfonyl chloride (1.06 g, 4.8 mmol) in dichloromethane (5 mL) was added dropwise to a cooled (-10° C.) stirred solution of Example 6a, Part B amine (1.05 g, 3.02 mmol) and triethyl amine (1.44 mL, 9.6 mmol) in dichloromethane (15 mL). After a few minutes, a precipitate formed. The suspension was stirred at -10° C. for 2.5 hours, diluted with dichloromethane (35 mL) and washed with 1N HCl solution (2×15 mL). The dichloromethane solution was dried (MgSO4), filtered and the solvent was removed in vacuo. The crude oil was purified on silica gel (Merck, 150 mL) eluting with 50% ethyl acetate in hexane to give title compound as a white foam (1.160 g, 72%).

후처리

  1. waitAfter a few minutes
  2. customa precipitate formed
  3. washwashed with 1N HCl solution (2×15 mL)
  4. dry with materialThe dichloromethane solution was dried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent was removed in vacuo
  7. customThe crude oil was purified on silica gel (Merck, 150 mL)
  8. washeluting with 50% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-eeedfc74393742b89ba7008c64e57f6a
출처 데이터셋
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05741792

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