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

HRID 376419ノート

反応式

HRID 376419 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 867518551,3-Dioleyloxy-2-propyl azide収率 100.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7906eb127ba54c5cb16618db4b4d388d
出典データセット
uspto-grants-2000_02
特許番号
US06020317

反応ノート

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