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Triethylamine → HCID 22843271, 화합물

HRID 1029649
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HRID 1029649 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:12][C@H:11]([OH:13])[CH2:10][C@H:9]1[CH3:14])=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:15][S:16](Cl)(=[O:18])=[O:17].C(N(CC)CC)C>ClCCl>[C:1]([O:5][C:6]([N:8]1[CH2:12][C@H:11]([O:13][S:16]([CH3:15])(=[O:18])=[O:17])[CH2:10][C@H:9]1[CH3:14])=[O:7])([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 14117010tert-butyl (2R,4R)-4-hydroxy-2-methylpyrrolidine-1-carboxylate

생성물 1

HCID 22843271HCID 22843271, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of (2R,4R)-1-(tert-butoxycarbonyl)-4-hydroxy-2-methylpyrrolidine (1.92 g) and methanesulfonyl chloride (955 μl) in dichloromethane (30 ml) was added dropwise triethylamine (1.99 ml) at 0° C. After one hour, the reaction mixture was washed in turn with 1N-hydrochloric acid and brine and the organic layer was dried over magnesium sulfate. Evaporation of the solvent gave an oil, which was chromatographed on silica gel (200 ml) eluting with a mixture of hexane and ethyl acetate (1:1, V/V) to give (2R,4R)-1-(tert-butoxycarbonyl)-4-methanesulfonyloxy-2-methylpyrrolidine (2.49 g).

후처리

  1. washthe reaction mixture was washed in turn with 1N-hydrochloric acid and brine
  2. dry with materialthe organic layer was dried over magnesium sulfate
  3. customEvaporation of the solvent
  4. customgave an oil, which
  5. customwas chromatographed on silica gel (200 ml)
  6. washeluting with a mixture of hexane and ethyl acetate (1:1, V/V)

출처 및 근거

ORD 기록
ord-6c30f1ff030646268a616c82e032db54
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05102877

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