HCID 70195797, 화합물 → 3-Bromomethyl-7-phenylacetamido-3-cephem-4-carboxylic acid-1-oxide

HRID 67962노트

반응식

HRID 67962 반응식
[Br:1][CH2:2][C:3]1[CH2:4][S:5](=[O:29])[C@@H:6]2[CH:17]([NH:18][C:19](=[O:27])[CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:16](=[O:28])[N:7]2[C:8]=1[C:9]([O:11]C(C)(C)C)=[O:10]>FC(F)(F)C(O)=O>[Br:1][CH2:2][C:3]1[CH2:4][S:5](=[O:29])[C@@H:6]2[CH:17]([NH:18][C:19](=[O:27])[CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:16](=[O:28])[N:7]2[C:8]=1[C:9]([OH:11])=[O:10]

참가 물질

3

반응물 1

HCID 70195797HCID 70195797, 화합물

생성물 1

HCID 679284423-Bromomethyl-7-phenylacetamido-3-cephem-4-carboxylic acid-1-oxide수율 102.2%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of 37.3 g of t-butyl 3-bromomethyl-7-phenylacetamido-3-cephem-4-carboxylate-1-oxide in 130 ml of trifluoroacetic acid was stirred for 15 minutes at room temperature and then the solvent was removed by evaporation under vacuo. After addition of 100 ml of 1,2-dichloroethane, evaporation to dryness was repeated. Ether was added to the residue and the crystals were vacuum filtered, washed with ether and dried under vacuo to obtain 33.7 g of 3-bromomethyl-7-phenylacetamido-3-cephem-4-carboxylic acid-1-oxide as an almost colorless solid having the following characteristics:

후처리

  1. customthe solvent was removed by evaporation under vacuo
  2. additionAfter addition of 100 ml of 1,2-dichloroethane, evaporation to dryness
  3. additionEther was added to the residue
  4. filtrationfiltered
  5. washwashed with ether
  6. customdried under vacuo

출처 및 근거

ORD 기록
ord-dec68ae2819140e6b643d81d63ad9589
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04347358

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