Methane → Sodium 3-chloro-1-azabicyclo[3.2.0]hept-2-en-7-one-2-carboxylate

HRID 1105862노트

반응식

HRID 1105862 반응식
[Cl:1][C:2]1[CH2:8][CH:7]2[N:4]([C:5](=[O:9])[CH2:6]2)[C:3]=1[C:10]([O:12]CC1C=CC=CC=1)=[O:11].C(=O)(O)[O-].[Na+:24].C>CO.O.[Pd]>[Cl:1][C:2]1[CH2:8][CH:7]2[N:4]([C:5](=[O:9])[CH2:6]2)[C:3]=1[C:10]([O-:12])=[O:11].[Na+:24]

참가 물질

7

반응물 3

HCID 297MethaneHCID 516892Sodium BicarbonateHCID 12804728Benzyl 3-chloro-1-azabicyclo[3.2.0]hept-2-en-7-one-2carboxylate

생성물 1

HCID 23672728Sodium 3-chloro-1-azabicyclo[3.2.0]hept-2-en-7-one-2-carboxylate

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 962Water용매

실험 절차

Benzyl 3-chloro-1azabicyclo[3.2.0]hept-2-en-7-one-2-carboxylate (28 mg) in methanol (2.5 ml) and water (0.5 ml) containing sodium bicarbonate (8.5 ml) is hydrogenated with 10% palladium on powdered charcoal (30 mg) at 40 psi for 30 minutes. The mixture is filtered and the catalyst is washed with water (5 ml). The combined filtrate is concentrated in vacuo to 1/2 its volume, washed with ethylacetate, and lyophilized to provide sodium 3-chloro-1-azabicyclo[3.2.0]hept-2-en-7-one-2-carboxylate.

후처리

  1. filtrationThe mixture is filtered
  2. washthe catalyst is washed with water (5 ml)
  3. concentrationThe combined filtrate is concentrated in vacuo to 1/2 its volume
  4. washwashed with ethylacetate

출처 및 근거

ORD 기록
ord-7259b4d899b34af1a6789e283ddcee46
출처 데이터셋
uspto-grants-1982_01
특허 번호
US04310538

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