Triphenylphosphine → (3,4,5-Tribromo-2-thenyl)triphenylphosphonium chloride

HRID 904450

反応式

HRID 904450 の反応式
[C:1]1([P:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Br:20][C:21]1[C:25]([Br:26])=[C:24]([Br:27])[S:23][C:22]=1[CH2:28][Cl:29]>C1(C)C=CC=CC=1>[Cl-:29].[Br:20][C:21]1[C:25]([Br:26])=[C:24]([Br:27])[S:23][C:22]=1[CH2:28][P+:7]([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 11776TriphenylphosphineHCID 151249082,3,4-Tribromo-5-(chloromethyl)thiophene

生成物 1

HCID 20285678(3,4,5-Tribromo-2-thenyl)triphenylphosphonium chloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Triphenylphosphine (9.0 g.) and 10.4 g. of 3,4,5-tribromo-2-chloromethylthiophene were dissolved in 200 ml. of toluene. The mixture was refluxed overnight under argon, cooled to room temperature and the precipitated phosphonium salt was collected by filtration, washed several times with cold benzene and dried at 80° C. under high vacuum. The resulting (3,4,5-tribromo-2-thenyl)triphenylphosphonium chloride has a m.p. 248°-249° C.

後処理

  1. temperatureThe mixture was refluxed overnight under argon
  2. filtrationthe precipitated phosphonium salt was collected by filtration
  3. washwashed several times with cold benzene
  4. customdried at 80° C. under high vacuum

出典と根拠

ORDレコード
ord-784c2b5116a447119fb3b025dce51292
出典データセット
uspto-grants-1980_10
特許番号
US04230872

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