Tert-Butylamine → (S)-3-(tert-Butylamino)propane-1,2-diol

HRID 2289169

반응식

HRID 2289169 반응식
[CH2:1]1[O:3][C@H:2]1[CH2:4][OH:5].[C:6]([NH2:10])([CH3:9])([CH3:8])[CH3:7]>O>[C:6]([NH:10][CH2:1][C@H:2]([OH:3])[CH2:4][OH:5])([CH3:9])([CH3:8])[CH3:7]

참가 물질

4

반응물 2

HCID 6385Tert-ButylamineHCID 6973630(-)-Glycidol

생성물 1

HCID 2733671(S)-3-(tert-Butylamino)propane-1,2-diol수율 78%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

(S)-Glycidol was added dropwise, with stirring, to a mixture of 54.7 g of tert-butylamine and 25 mL of water, heated at reflux. The resulting mixture was heated at reflux for 12 h, and was thereafter allowed to cool to room temperature. The mixture was concentrated in vacuo and was treated with ether to effect crystallization. 28.6 g (78%) of crystalline product was thus obtained: 1H NMR (CDCl3) δ1.0 (s, C(CH3)3), 2.4-2.6 (m), 3.3-4.2 (m); 13C NMR (CDCl3) δ28.6 (3 CH3), 45.2 (CH2NH), 50.2 (C(CH3)3), 65.5 (CH2OH), 70.6 (CHOH).

후처리

  1. temperatureheated
  2. temperatureat reflux
  3. temperatureThe resulting mixture was heated
  4. temperatureat reflux for 12 h
  5. concentrationThe mixture was concentrated in vacuo
  6. additionwas treated with ether
  7. customcrystallization

출처 및 근거

ORD 기록
ord-9aa4c8d18b434bbea59198306eded1ee
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06090950

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