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Dimethylamine → ((S)-1-dimethylaminomethyl-3,3-dimethyl-butyl)-carbamic acid tert-butyl ester

HRID 1879460
ノート
印刷プレビュー

反応式

HRID 1879460 の反応式
[CH3:1][NH:2][CH3:3].[C:4]([O:8][C:9]([NH:11][C@@H:12]([CH2:25][C:26]([CH3:29])([CH3:28])[CH3:27])[CH2:13]OS(C1C=CC(C)=CC=1)(=O)=O)=[O:10])([CH3:7])([CH3:6])[CH3:5]>N1C=CC=CC=1.[OH-].[K+]>[C:4]([O:8][C:9](=[O:10])[NH:11][C@H:12]([CH2:13][N:2]([CH3:3])[CH3:1])[CH2:25][C:26]([CH3:29])([CH3:28])[CH3:27])([CH3:7])([CH3:6])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 674DimethylamineHCID 58280488toluene-4-sulfonic acid (S)-2-tert-butoxycarbonylamino-4,4-dimethyl-pentyl ester

生成物 1

HCID 58280493((S)-1-dimethylaminomethyl-3,3-dimethyl-butyl)-carbamic acid tert-butyl ester収率 65.2%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 14797Potassium Hydroxide溶媒

実験手順

Dimethylamine (11.2 g, 249.3 mmol, 30.0 equiv) was added portionwise to a stirred solution of toluene-4-sulfonic acid(S)-2-tert-butoxycarbonylamino-4,4-dimethyl-pentyl ester (3.2 g, 8.31 mmol, 1.0 equiv.) in pyridine (9.6 mL) at 0° C. The reaction mixture was slowly warmed to room temperature and stirred for an additional 20 hours at the same temperature. The reaction mixture was diluted with the addition of an aqueous solution of 10% potassium hydroxide (w/v; 30 mL) and was extracted with dichloromethane (3×150 mL). The collected organic extracts were dried over anhydrous sodium sulfate, concentrated under reduced pressure to obtain a crude mass. This was purified by purified by silica gel column chromatography (100-200 mesh) using a gradient of 2-5% methanol/dichloromethane to give ((S)-1-dimethylaminomethyl-3,3-dimethyl-butyl)-carbamic acid tert-butyl ester (1.4 g, 65%).

後処理

  1. extractionwas extracted with dichloromethane (3×150 mL)
  2. dry with materialThe collected organic extracts were dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customto obtain a crude mass
  5. customThis was purified
  6. customby purified by silica gel column chromatography (100-200 mesh)

出典と根拠

ORDレコード
ord-3b116bd77e954d97ae2d9c88fd99ca7d
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08314250B2

反応ノート

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