Diazomethane → HCID 70500625, 화합물

HRID 1902906노트

반응식

HRID 1902906 반응식
[N+](=[CH2:3])=[N-].[C:4]([NH:12][CH:13]1[C:25](=[O:26])[N:15]2[C:16]([C:22]([OH:24])=[O:23])=[C:17]([CH3:21])[CH2:18][S:19](=[O:20])[C@H:14]12)(=[O:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>ClCCl>[C:4]([NH:12][CH:13]1[C:25](=[O:26])[N:15]2[C:16]([C:22]([O:24][CH3:3])=[O:23])=[C:17]([CH3:21])[CH2:18][S:19](=[O:20])[C@H:14]12)(=[O:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

참가 물질

4

반응물 2

HCID 9550DiazomethaneHCID 704647027-Benzamido-3-methyl-3-cephem-4-carboxylic acid-1-oxide

생성물 1

HCID 70500625HCID 70500625, 화합물수율 86.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

An excess of an ethereal diazomethane solution was added to an ice-cooled suspension of 5 gm of 7-benzamido-3-methyl-3-cephem-4-carboxylic acid-1-oxide in 150 ml of dichloromethane and the mixture was stirred for half an hour. Then, excess diazomethane was destroyed with acetic acid and methanol was added. The mixture was evaporated to dryness in vacuo and the residue was crystallized from methanol to obtain 4.5 gm (86.6% yield) of methyl 7-benzamido-3-methyl-3-cephem-4-carboxylate-1-oxide.

후처리

  1. temperaturecooled
  2. customThen, excess diazomethane was destroyed with acetic acid and methanol
  3. additionwas added
  4. customThe mixture was evaporated to dryness in vacuo
  5. customthe residue was crystallized from methanol

출처 및 근거

ORD 기록
ord-71dbe44d8fb844349aab7616008a9569
출처 데이터셋
uspto-grants-1982_12
특허 번호
US04366315

반응 노트

불러오는 중…