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Sodium Hydroxide → HCID 57893118、化合物

HRID 1511455
ノート
印刷プレビュー

反応式

HRID 1511455 の反応式
C([O:4][CH:5]([C@@H:12]([NH:18][C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:13][CH:14]1[CH2:17][CH2:16][CH2:15]1)[C:6]([NH:8][CH:9]1[CH2:11][CH2:10]1)=[O:7])(=O)C.[OH-].[Na+]>CO>[CH:14]1([CH2:13][C@H:12]([NH:18][C:19](=[O:20])[O:21][C:22]([CH3:24])([CH3:23])[CH3:25])[CH:5]([OH:4])[C:6]([NH:8][CH:9]2[CH2:10][CH2:11]2)=[O:7])[CH2:17][CH2:16][CH2:15]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 57893114(3S)-3-(tert-butoxycarbonylamino)-4-cyclobutyl-1-(cyclopropylamino)-1-oxobutan-2-yl acetate

生成物 1

HCID 57893118HCID 57893118、化合物収率 86.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of (3S)-3-(tert-butoxycarbonylamino)-4-cyclobutyl-1-(cyclopropylamino)-1-oxobutan-2-yl acetate (3.8 g, 10.7 mmol) in methanol (50 mL) was added sodium hydroxide aqueous solution (1N, 15 mL) at room temperature. After 2 hours, methanol was removed under reduced pressure, and the concentrate was extracted with ethyl acetate. The ethyl acetate was washed with brine and dried over magnesium sulfate. The solvent was removed under reduced pressure, and the residue was crystallized from 100 mL of ethyl acetate and hexane(v/v=3/1) to give tert-butyl (2S)-1-cyclobutyl-4-(cyclopropylamino)-3-hydroxy-4-oxobutan-2-ylcarbamate (2.9 g) as a white solid.

後処理

  1. custommethanol was removed under reduced pressure
  2. extractionthe concentrate was extracted with ethyl acetate
  3. washThe ethyl acetate was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was crystallized from 100 mL of ethyl acetate and hexane(v/v=3/1)

出典と根拠

ORDレコード
ord-8c8c298723ee4e1db462305b31f299cd
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08211897B2

反応ノート

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