Lithium azide → 1,3-Dioleyloxy-2-propyl azide

HRID 376419노트

반응식

HRID 376419 반응식
[CH2:1]([O:19][CH2:20][CH:21]([CH2:33][O:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42]/[CH:43]=[CH:44]\[CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][CH3:52])OS(C1C=CC(C)=CC=1)(=O)=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]/[CH:9]=[CH:10]\[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].[N-:53]=[N+:54]=[N-:55].[Li+]>CN(C)C=O>[CH2:1]([O:19][CH2:20][CH:21]([N:53]=[N+:54]=[N-:55])[CH2:33][O:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42]/[CH:43]=[CH:44]\[CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][CH3:52])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]/[CH:9]=[CH:10]\[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]

참가 물질

4

반응물 2

HCID 88163Lithium azideHCID 867518541,3-O-dioleyl-2-O-(p-toluenesulfonyl)glycerol

생성물 1

HCID 867518551,3-Dioleyloxy-2-propyl azide수율 100.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

A mixture of 150 mg (80%) of the above 1,3-O-dioleyl-2-O-(p-toluenesulfonyl)glycerol, 30 mg (0.6 mmol) of lithium azide, and 5 ml of N,N-dimethylformamide was stirred at 100 ° C. for 2 hours. After cooling, the solvent was distilled off and the residue was diluted with water and extracted with ether. The extract was washed with water, dried, and concentrated to provide 125 mg (99%) of 1,3-dioleyloxy-2-propyl azide as light-brown oil.

후처리

  1. temperatureAfter cooling
  2. distillationthe solvent was distilled off
  3. additionthe residue was diluted with water
  4. extractionextracted with ether
  5. washThe extract was washed with water
  6. customdried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-7906eb127ba54c5cb16618db4b4d388d
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06020317

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