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

HRID 1105862ノート

反応式

HRID 1105862 の反応式
[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]

参加物

7

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7259b4d899b34af1a6789e283ddcee46
出典データセット
uspto-grants-1982_01
特許番号
US04310538

反応ノート

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