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Anaesthaminol → Ethyl 2-(3-chloropropyl)-5-benzoxazolecarboxylate

HRID 1195665
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HRID 1195665 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][C:12]=1[OH:13])[C:5]([O:7][CH2:8][CH3:9])=[O:6].Cl.[Cl:15][CH2:16][CH2:17][CH2:18][C:19](=N)OCC>ClC(Cl)Cl>[Cl:15][CH2:16][CH2:17][CH2:18][C:19]1[O:13][C:12]2[CH:11]=[CH:10][C:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])=[CH:3][C:2]=2[N:1]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 12208891AnaesthaminolHCID 13163359Ethyl 4-chlorobutanimidate hydrochloride

생성물 1

HCID 54024397Ethyl 2-(3-chloropropyl)-5-benzoxazolecarboxylate수율 74.7%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
20 °C

실험 절차

A mixture of 9 parts of ethyl 3-amino-4-hydroxybenzoate, 10.2 parts of ethyl 4-chlorobutanimidate hydrochloride and 150 parts of trichloromethane was stirred for 24 hours at 20° C. The separated organic layer was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (98:2 by volume) as eluent. The eluent of the desired fraction was evaporated, yielding 10 parts (74.7%) of ethyl 2-(3-chloropropyl)-5-benzoxazolecarboxylate as a residue (interm. 25).

후처리

  1. customThe separated organic layer was dried
  2. filtrationfiltered
  3. customevaporated
  4. customThe residue was purified by column chromatography over silica gel using
  5. additiona mixture of trichloromethane and methanol (98:2 by volume) as eluent
  6. customThe eluent of the desired fraction was evaporated

출처 및 근거

ORD 기록
ord-6d13d5a73a284bd9be619e46b9c4caa2
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05112825

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