Methane → Sodium 6-(2,2,2-trifluoro-1-hydroxyethyl)-3-morpholino-1-azabicyclo[3.2.0]hept-2-en-7-one-2-carboxylate

HRID 247490ノート

反応式

HRID 247490 の反応式
[F:1][C:2]([F:30])([F:29])[CH:3]([CH:5]1[C:11](=[O:12])[N:10]2[CH:6]1[CH2:7][C:8]([N:23]1[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1)=[C:9]2[C:13]([O:15]CC1C=CC=CC=1)=[O:14])[OH:4].C.C(=O)(O)[O-].[Na+:36].O1CCOCC1>[Pd].O>[F:30][C:2]([F:1])([F:29])[CH:3]([CH:5]1[C:11](=[O:12])[N:10]2[CH:6]1[CH2:7][C:8]([N:23]1[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1)=[C:9]2[C:13]([O-:15])=[O:14])[OH:4].[Na+:36]

参加物

7

反応物 4

HCID 297MethaneHCID 312751,4-DioxaneHCID 516892Sodium BicarbonateHCID 20160992Benzyl 6-(2,2,2-trifluoro-1-hydroxyethyl)-3-morpholino-1-azabicyclo[3.2.0]hept-2-en-7-one-2-carboxylate

生成物 1

HCID 23674972Sodium 6-(2,2,2-trifluoro-1-hydroxyethyl)-3-morpholino-1-azabicyclo[3.2.0]hept-2-en-7-one-2-carboxylate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

実験手順

A mixture of benzyl 6-(2,2,2-trifluoro-1-hydroxyethyl)-3-morpholino-1-azabicyclo[3.2.0]hept-2-en-7-one-2-carboxylate (25 mg), 10% palladium on powdered charcoal (25 mg), sodium bicarbonate (5 mg), dioxane (2 ml), and water (1 ml) is hydrogenated at 40 psi for 30 mins. The mixture is filtered to remove the catalyst which is washed with water (3×2 ml). The combined filtrate is extracted with ethyl acetate (2×2 ml), concentrated in vacuo, and lyophilized to give sodium 6-(2,2,2-trifluoro-1-hydroxyethyl)-3-morpholino-1-azabicyclo[3.2.0]hept-2-en-7-one-2-carboxylate.

後処理

  1. filtrationThe mixture is filtered
  2. customto remove the catalyst which
  3. washis washed with water (3×2 ml)
  4. extractionThe combined filtrate is extracted with ethyl acetate (2×2 ml)
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2aac9ae023e44af898fd1d2e293e4f1b
出典データセット
uspto-grants-1987_11
特許番号
US04707547

反応ノート

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