Trifluoroacetic acid → HCID 20314460、化合物

HRID 973311ノート

反応式

HRID 973311 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:18]=[CH:17][C:16]([I:19](OC(=O)C)OC(=O)C)=[CH:15][CH:14]=2)=[CH:9][CH:8]=1.[F:28][C:29]([F:34])([F:33])[C:30]([OH:32])=[O:31]>C(OC(=O)C)(=O)C>[F:28][C:29]([F:34])([F:33])[C:30]([O-:32])=[O:31].[Cl:6][C:7]1[CH:8]=[CH:9][C:10]([C:13]2[CH:18]=[CH:17][C:16]([I+:19][C:2]3[S:1][CH:5]=[CH:4][CH:3]=3)=[CH:15][CH:14]=2)=[CH:11][CH:12]=1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 8030ThiopheneHCID 20314474HCID 20314474、化合物

生成物 1

HCID 20314460HCID 20314460、化合物

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒2 回

反応条件

温度
-10 °C

実験手順

A mixture of thiophene (8.7 g.) and acetic anhydride (60 ml.) is added to a stirred suspension of 4-(4-chlorophenyl)-(diacetoxyiodo)benzene (21.7 g.) in a mixture of acetic anhydride (50 ml.) and trifluoroacetic acid (15 ml.) below -10° C. during 1 hour. The mixture is stirred at -10° C. for 2 hours, at ambient temperature for 18 hours and is then filtered. The filtrate is concentrated to small volume in vacuo, and ether is added. The solid so formed is filtered off and crystallised from toluene to give 4-(4-chlorophenyl)-phenyl-2-thienyliodonium trifluoroacetate (13.7 g.), m.p. 175°-177° C.

後処理

  1. filtrationis then filtered
  2. concentrationThe filtrate is concentrated to small volume in vacuo, and ether
  3. additionis added
  4. customThe solid so formed
  5. filtrationis filtered off
  6. customcrystallised from toluene

出典と根拠

ORDレコード
ord-07508b027d284a738035660ac5d141f6
出典データセット
uspto-grants-1977_10
特許番号
US04055595

反応ノート

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