Triethylamine → 1-Benzyloxycarbonylamino-3-methoxy-2-propanol

HRID 1729320노트

반응식

HRID 1729320 반응식
C(N(CC)CC)C.[NH2:8][CH2:9][CH:10]([OH:14])[CH2:11][O:12][CH3:13].[CH2:15]([O:22][C:23](Cl)=[O:24])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>O1CCCC1.C(OCC)(=O)C>[CH2:15]([O:22][C:23]([NH:8][CH2:9][CH:10]([OH:14])[CH2:11][O:12][CH3:13])=[O:24])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 1245101-Amino-3-methoxypropan-2-ol

생성물 1

HCID 190124911-Benzyloxycarbonylamino-3-methoxy-2-propanol수율 56.7%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

19.69 g of triethylamine are added to a solution of 10.23 g of 1-amino-3- methoxy-2-propanol in 100 ml of tetrahydrofuran. After the mixture is cooled, a solution of 16.60 g of benzyloxycarbonyl chloride in 50 ml of tetrahydrofuran is added dropwise thereto for 30 minutes. The mixture is stirred at room temperature for one hour. The reaction mixture is diluted with ethyl acetate, washed with water and dried. The residue is purified by silica gel column chromatography [solvent: ethyl acetate - hexane (2:1)]. 13.2 g of 1-benzyloxycarbonylamino-3- methoxy-2-propanol are obtained as colorless oil.

후처리

  1. temperatureAfter the mixture is cooled
  2. washwashed with water
  3. customdried
  4. customThe residue is purified by silica gel column chromatography [solvent: ethyl acetate - hexane (2:1)]

출처 및 근거

ORD 기록
ord-7a671331d9fe4131b211b8303ad558e2
출처 데이터셋
uspto-grants-1994_07
특허 번호
US05332754

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