Trifluoroacetic acid → HCID 20314460, 화합물

HRID 973311노트

반응식

HRID 973311 반응식
[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

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 8030ThiopheneHCID 20314474HCID 20314474, 화합물

생성물 1

HCID 20314460HCID 20314460, 화합물

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매2회

반응 조건

온도
-10 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-07508b027d284a738035660ac5d141f6
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04055595

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