HCID 70195797、化合物 → 3-Bromomethyl-7-phenylacetamido-3-cephem-4-carboxylic acid-1-oxide

HRID 67962ノート

反応式

HRID 67962 の反応式
[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]

参加物

3

反応物 1

HCID 70195797HCID 70195797、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-dec68ae2819140e6b643d81d63ad9589
出典データセット
uspto-grants-1982_08
特許番号
US04347358

反応ノート

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