4-Amino-1-butanol → 4-Tert-butoxycarbonylmethylamino-1-butanol

HRID 18017

反応式

HRID 18017 の反応式
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][NH2:6].Br[CH2:8][C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10]>C(OCC)C>[C:12]([O:11][C:9](=[O:10])[CH2:8][NH:6][CH2:5][CH2:4][CH2:3][CH2:2][OH:1])([CH3:15])([CH3:14])[CH3:13]

参加物

4

反応物 2

HCID 258684-Amino-1-butanolHCID 79177tert-Butyl bromoacetate

生成物 1

HCID 108458284-Tert-butoxycarbonylmethylamino-1-butanol

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a cold (0° C.) solution of 4-hydroxybutylamine (9.1 g, 101.8 mmol) in diethyl ether (100 mL), a solution of tert-butyl bromoacetate (7.4 g, 49.3 mmol) in diethyl ether (25 mL) was added dropwise over a period of 2 hours. The reaction mixture was allowed to warm up slowly to room temperature and stirred at the temperature overnight. The product mixture was washed successively with aqueous NaHCO3, water, and brine. The organic extract was dried over anhydrous sodium sulfate, filtered, and concentrated under vacuum. This intermediate was used in the following reaction without further purification.

後処理

  1. washThe product mixture was washed successively with aqueous NaHCO3, water, and brine
  2. extractionThe organic extract
  3. dry with materialwas dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum
  6. customThis intermediate was used in the following reaction without further purification

出典と根拠

ORDレコード
ord-301a1819b29342888da55e194bb046f4
出典データセット
uspto-grants-2010_06
特許番号
US07741315B2

関連ノート

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