Phosphorus trichloride → 3-tert-Butyl-2-chloro-1,3,2-oxazaphospholidine

HRID 580062노트

반응식

HRID 580062 반응식
[P:1]([Cl:4])(Cl)Cl.[C:5]([NH:9][CH2:10][CH2:11][OH:12])([CH3:8])([CH3:7])[CH3:6]>C1(C)C=CC=CC=1>[C:5]([N:9]1[CH2:10][CH2:11][O:12][P:1]1[Cl:4])([CH3:8])([CH3:7])[CH3:6]

참가 물질

4

반응물 2

HCID 24387Phosphorus trichlorideHCID 783612-(tert-Butylamino)ethanol

생성물 1

HCID 142281093-tert-Butyl-2-chloro-1,3,2-oxazaphospholidine수율 56.7%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a solution of 8.7 ml (0.10 mol) of phosphorus trichloride in 200 ml of toluene in a 500 ml three neck flask equipped with a mechanical stirrer, a condenser and an addition funnel is added a solution of 11.72 g (0.10 mol) of 2-tert-butylaminoethanol in 50 ml of toluene. After refluxing for 16 hours, the orange solids are filtered off and the filtrate concentrated in vacuo. Distillation under reduced pressure gives 10.3 g (56.7%) of clear liquid: b.p. 82° C./1.0 mm Hg.

후처리

  1. temperatureAfter refluxing for 16 hours
  2. filtrationthe orange solids are filtered off
  3. concentrationthe filtrate concentrated in vacuo
  4. distillationDistillation under reduced pressure

출처 및 근거

ORD 기록
ord-d90bf00b6db3461c920f45f5ffc667a9
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04751319

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