Sodium Azide → 3-Azido-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one

HRID 482721

反応式

HRID 482721 の反応式
Cl[CH:2]1[CH2:8][CH2:7][C:6]2[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=2[NH:4][C:3]1=[O:13].[N-:14]=[N+:15]=[N-:16].[Na+]>CS(C)=O>[N:14]([CH:2]1[CH2:8][CH2:7][C:6]2[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=2[NH:4][C:3]1=[O:13])=[N+:15]=[N-:16]

参加物

4

反応物 2

HCID 33557Sodium AzideHCID 132434963-Chloro-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one

生成物 1

HCID 109325203-Azido-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A solution of 3-chloro-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one (15.9 g, 0.08 mol) and sodium azide (6.36 g, 0.10 mol) in dimethylsulfoxide (320 ml) was maintained at 80° C. under an atmosphere of nitrogen for 3 hours. At this time, the IR spectrum of an aliquot showed a strong peak at 2150 cm-1 characteristic of the azide group. The reaction mixture was poured into 1000 ml of ice/water and the suspension was stirred for 30 min. The solid was filtered off, washed with water (250 ml) and dried to give 3-azido-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one, m.p. 142°-5°.

後処理

  1. filtrationThe solid was filtered off
  2. washwashed with water (250 ml)
  3. customdried

出典と根拠

ORDレコード
ord-b3ddd47261bc4bafbec1eb97ce293cbb
出典データセット
uspto-grants-1986_03
特許番号
US04575503

関連ノート

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