Isocyanate → HCID 10573917、化合物

HRID 1977734ノート

反応式

HRID 1977734 の反応式
[Br:1][C:2]1[CH:3]=[C:4](C(N=[N+]=[N-])=O)[CH:5]=[N:6][CH:7]=1.[N-:13]=[C:14]=[O:15].[CH3:16][O:17][C:18]1[CH:19]=[C:20]2[C:24](=[CH:25][C:26]=1[C:27]([F:30])([F:29])[F:28])[NH:23][CH2:22][CH2:21]2>C1(C)C=CC=CC=1.ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([NH:13][C:14]([N:23]2[C:24]3[C:20](=[CH:19][C:18]([O:17][CH3:16])=[C:26]([C:27]([F:29])([F:30])[F:28])[CH:25]=3)[CH2:21][CH2:22]2)=[O:15])[CH:5]=[N:6][CH:7]=1

参加物

6

反応物 3

HCID 105034IsocyanateHCID 112067135-Methoxy-6-(trifluoromethyl)indolineHCID 156228505-Bromopyridine-3-carbonyl azide

生成物 1

HCID 10573917HCID 10573917、化合物収率 81%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

実験手順

5-Bromo-3-pyridylcarbonylazide (3.7 g, 16 mmoles) was heated under reflux in dry toluene (100 ml) for 1 hr. After cooling the resulting solution of isocyanate was treated with a solution of 5-methoxy-6-trifluoromethyl indoline (D11) (3.5 g, 16 mmoles) in dichloromethane (600 ml) and stirred overnight. The mixture was concentrated in vacuo and the residue triturated with diethyl ether. Filtration and washing with more diethyl ether gave the title compound (D26) (5.4 g, 81%).

後処理

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue triturated with diethyl ether
  3. filtrationFiltration
  4. washwashing with more diethyl ether

出典と根拠

ORDレコード
ord-cc56efc174944a089ddd93295700c01d
出典データセット
uspto-grants-2001_05
特許番号
US06235758B1

反応ノート

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