Sodium Hydroxide → HCID 67490897、化合物

HRID 1917370ノート

反応式

HRID 1917370 の反応式
[OH-].[Na+].C[O:4][C:5]([C:7]12[CH2:14][CH2:13][CH:12]=[C:11]1[CH2:10][N:9]([C:15]([O:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:16])[CH2:8]2)=[O:6]>CO>[CH2:18]([O:17][C:15]([N:9]1[CH2:10][C:11]2[C:7]([C:5]([OH:6])=[O:4])([CH2:14][CH2:13][CH:12]=2)[CH2:8]1)=[O:16])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 67490992HCID 67490992、化合物

生成物 1

HCID 67490897HCID 67490897、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 1N sodium hydroxide solution (1.86 mL) was added to a solution of {3-benzyloxycarbonyl-3-azabicyclo[3.3.0]oct-5-en-1-yl}carboxylic acid methyl ester (187 mg, 0.620 mmol) in methanol (6.20 mL) in a nitrogen atmosphere, and the mixture was stirred at room temperature for 16 hours. The reaction solution was concentrated under reduced pressure and then washed with diethyl ether (50 mL×2). The aqueous layer was made acidic with 1N hydrochloric acid under ice-cooling, followed by extraction with ethyl acetate (100 mL×1, 80 mL×1). The organic layer was washed with water (80 mL) and brine (80 mL) and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure to give 186 mg (quantitative) of the title compound.

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. washwashed with diethyl ether (50 mL×2)
  3. temperaturecooling
  4. extractionfollowed by extraction with ethyl acetate (100 mL×1, 80 mL×1)
  5. washThe organic layer was washed with water (80 mL) and brine (80 mL)
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationAfter filtration
  8. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-f81bd2e0f9024a2b86ed0729f8a26cfd
出典データセット
uspto-grants-2013_12
特許番号
US08618094B2

反応ノート

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