Sodium Azide → 2-Azido-5-chloro-2'-fluorobenzophenone

HRID 267548

反応式

HRID 267548 の反応式
[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:5].N([O-])=O.[Na+].C([O-])(=O)C.[Na+].[N-:27]=[N+:28]=[N-].[Na+]>C(O)(=O)C.Cl.O>[N:1]([C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:5])=[N+:27]=[N-:28]

参加物

8

反応物 4

HCID 33557Sodium AzideHCID 699122-Amino-5-chloro-2'-fluorobenzophenoneHCID 517045Sodium AcetateHCID 23668193Sodium Nitrite

生成物 1

HCID 215549972-Azido-5-chloro-2'-fluorobenzophenone

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

10 G (0.04 mol) of 2-amino-5-chloro-2'-fluorobenzophenone are dissolved in a mixture of 40 ml of glacial acetic acid and 10 ml of concentrated hydrochloric acid and diazotised with 10 ml (0.04 mol) of 4 M sodium nitrite solution. The mixture is then diluted with 200 ml of ice-cold water and neutralised by addition of 16.3 g (0.12 mol) of crystalline sodium acetate. The turbid solution is clarified by filtration using active charcoal and a solution of 8.5 g (0.13 mol) of sodium azide in 100 ml of water is then added. The reaction product which has precipitated is filtered off and washed with water until neutral. After drying over potassium hydroxide/calcium chloride in a desiccator, 2-azido-5-chloro-2'-fluorobenzophenone of decomposition point 90°C is obtained.

後処理

  1. filtrationThe turbid solution is clarified by filtration
  2. customThe reaction product which has precipitated
  3. filtrationis filtered off
  4. washwashed with water until neutral
  5. dry with materialAfter drying over potassium hydroxide/calcium chloride in a desiccator

出典と根拠

ORDレコード
ord-74449a8db68b4211b700be4941ae260f
出典データセット
uspto-grants-1976_03
特許番号
US03943145

関連ノート

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