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O-Methylhydroxylamine hydrochloride → HCID 131710493, 화합물

HRID 972488
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HRID 972488 반응식
CO[CH:3](OC)[C:4]1[CH2:5][S:6][C@@H:7]2[C@H:14]([NH:15][C:16](=[O:23])[CH2:17][C:18]3[S:19][CH:20]=[CH:21][CH:22]=3)[C:13](=[O:24])[N:8]2[C:9]=1[C:10]([OH:12])=[O:11].Cl.[CH3:28][O:29][NH2:30]>O1CCCC1.O>[CH3:28][O:29][N:30]=[CH:3][C:4]1[CH2:5][S:6][C@@H:7]2[C@H:14]([NH:15][C:16](=[O:23])[CH2:17][C:18]3[S:19][CH:20]=[CH:21][CH:22]=3)[C:13](=[O:24])[N:8]2[C:9]=1[C:10]([OH:12])=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 70636652HCID 70636652, 화합물

생성물 1

HCID 131710493HCID 131710493, 화합물수율 83.8%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 3-dimethoxymethyl-7β-(2-thienylacetamido)-3-cephem-4-carboxylic acid (76 mg) in tetrahydrofuran (4 ml) is added a solution of O-methylhydroxylamine hydrochloride (23 mg) in water (1 ml), and the mixture is kept at room temperature for 10 hours. The reaction mixture is evaporated to remove tetrahydrofuran, and the separated solid material is collected by filtration. Recrystallization of the solid from a mixture of ethyl acetate and ether gives 3-methoxyiminomethyl-7β-(2-thienylacetamido)-3-cephem-4-carboxylic acid (61 mg). m.p. 186°-189° C. Yield: 80%.

후처리

  1. customThe reaction mixture is evaporated
  2. customto remove tetrahydrofuran
  3. filtrationthe separated solid material is collected by filtration
  4. customRecrystallization of the solid
  5. additionfrom a mixture of ethyl acetate and ether

출처 및 근거

ORD 기록
ord-6d0a765fd1aa4336b0f0e2cd22c30767
출처 데이터셋
uspto-grants-1977_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04053469

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