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Diazomethane → HCID 12784140, 화합물

HRID 465172
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HRID 465172 반응식
[N+](=[CH2:3])=[N-].[N+:4]([C:7]1[CH:37]=[CH:36][C:10]([CH2:11][O:12][C:13]([C:15]2[N:20]3[C:21](=[O:34])[C@@H:22]([NH:23][C:24](=[O:33])[CH2:25][O:26][C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)[C@H:19]3[S:18][CH2:17][C:16]=2[OH:35])=[O:14])=[CH:9][CH:8]=1)([O-:6])=[O:5]>C(Cl)(Cl)Cl>[N+:4]([C:7]1[CH:8]=[CH:9][C:10]([CH2:11][O:12][C:13]([C:15]2[N:20]3[C:21](=[O:34])[C@@H:22]([NH:23][C:24](=[O:33])[CH2:25][O:26][C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)[C@H:19]3[S:18][CH2:17][C:16]=2[O:35][CH3:3])=[O:14])=[CH:36][CH:37]=1)([O-:6])=[O:5]
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참가 물질

4

반응물 2

HCID 9550DiazomethaneHCID 547167947beta-Phenoxyacetamido-3-hydroxy-3-cephem-4-carboxylic acid p-nitrobenzyl ester

생성물 1

HCID 12784140HCID 12784140, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
0 °C

실험 절차

3 ml of an ethereal diazomethane solution (0.5 molar, 1.5 equivalents) are added in the course of about 10 minutes to a solution, cooled to 0° C., of 485 mg of 7β-phenoxyacetamido-3-hydroxy-3-cephem-4-carboxylic acid p-nitrobenzyl ester in 10 ml of dry chloroform. The pale yellow solution is stirred for 1 hour at 0° C., flushed with nitrogen in order to remove excess diazomethane and concentrated in vacuo. The residue is recrystallised from methylene chloride and gives 7β-phenoxyacetamido-3-methoxy-3-cephem-4-carboxylic acid p-nitrobenzyl ester of melting point 140.5°-142° C.

후처리

  1. customflushed with nitrogen in order
  2. customto remove excess diazomethane
  3. concentrationconcentrated in vacuo
  4. customThe residue is recrystallised from methylene chloride

출처 및 근거

ORD 기록
ord-5c0d638caf224144be72a037b27d71dd
출처 데이터셋
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04550162

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