Sodium Chloride → HCID 13174771, 화합물

HRID 2109355노트

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HRID 2109355 반응식
[C:1]1([CH:7]([O:14][C:15]([CH:17]2[N:21]3[C:22](=[O:26])[C:23](Br)(Br)[C@H:20]3[S:19](=[O:27])[C:18]2([CH3:29])[CH3:28])=[O:16])[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Bi].[Cl-].[Na+].[Al]>ClCCl.CO>[C:1]1([CH:7]([O:14][C:15]([CH:17]2[N:21]3[C:22](=[O:26])[CH2:23][C@H:20]3[S:19](=[O:27])[C:18]2([CH3:29])[CH3:28])=[O:16])[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

7

반응물 4

HCID 5234Sodium ChlorideHCID 5359268AluminumHCID 5359367BismuthHCID 14096412HCID 14096412, 화합물3회

생성물 1

HCID 13174771HCID 13174771, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

반응 조건

온도
22.5 °C

실험 절차

A 86.6 g quantity of 6,6-dibromo-2,2-dimethylpenam-3-carboxylic acid 1-oxide diphenylmethyl ester (Compound 1) [compound of the formula (1) wherein X═Y═Br, R=diphenylmethyl, n=1] was dissolved in 300 mL of dichloromethane. To the solution was added 36 mL of methanol with stirring and then added a suspension of 1.05 g of metal bismuth in 112 mL of 20% aqueous solution of sodium chloride. While maintaining at 20 to 25° C., to the mixture was added 10 g of aluminum powder, each 1 g, at intervals of 10 minutes, thereafter the mixture was refluxed with heating. After 23.5 hours, the reaction mixture was cooled to room temperature, an organic layer was separated and washed with diluted hydrochloric acid and 5% aqueous solution of sodium chloride. The organic layer was concentrated to give 2,2-dimethylpenam-3-carboxylic acid 1-oxide diphenylmethyl ester (Compound 2) [compound of the formula (2) wherein R=diphenylmethyl, n=1].

후처리

  1. additionadded
  2. temperatureeach 1 g, at intervals of 10 minutes, thereafter the mixture was refluxed
  3. temperaturewith heating
  4. temperaturethe reaction mixture was cooled to room temperature
  5. customan organic layer was separated
  6. washwashed with diluted hydrochloric acid and 5% aqueous solution of sodium chloride
  7. concentrationThe organic layer was concentrated

출처 및 근거

ORD 기록
ord-34e8bbf76a3d4992877a8265a3b2797f
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07514553B2

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