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Triphenylphosphine → HCID 86744367、化合物

HRID 1110405
ノート
印刷プレビュー

反応式

HRID 1110405 の反応式
[Cl:1][CH2:2][CH:3]=[C:4]([CH:16]1[CH2:18][CH2:17]1)[C:5]1[CH:10]=[CH:9][C:8]([O:11][C:12]([F:15])([F:14])[F:13])=[CH:7][CH:6]=1.[C:19]1([P:25]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C1(C)C=CC=CC=1>[Cl-:1].[CH:16]1([C:4]([C:5]2[CH:10]=[CH:9][C:8]([O:11][C:12]([F:15])([F:14])[F:13])=[CH:7][CH:6]=2)=[CH:3][CH2:2][P+:25]([C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH2:18][CH2:17]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11776TriphenylphosphineHCID 537327453-Chloro-1-cyclopropyl-1-(4-trifluoromethoxyphenyl)-1-propene

生成物 1

HCID 86744367HCID 86744367、化合物収率 79.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A stirred solution of 113.5 grams (0.41 mole) of 3-chloro-1-cyclopropyl-1-(4-trifluoromethoxyphenyl)-1-propene and 113.0 grams (0.43 mole) of triphenylphosphine in 400 mL of toluene was heated at reflux for 4 hours. After this time the reaction mixture was cooled and concentrated under reduced pressure to a residue. The residue was triturated with 1000 mL of diethyl ether. The ether was decanted from the residue, and the residue was triturated with two more 1000 mL portions of diethyl ether in the manner described above. The solid residue was dried under reduced pressure yielding 176.0 grams of [3-cyclopropyl-3-(4-trifluoromethoxyphenyl)-2-propen-1-yl]triphenylphosphonium chloride.

後処理

  1. temperatureat reflux for 4 hours
  2. temperatureAfter this time the reaction mixture was cooled
  3. concentrationconcentrated under reduced pressure to a residue
  4. customThe residue was triturated with 1000 mL of diethyl ether
  5. customThe ether was decanted from the residue
  6. customthe residue was triturated with two more 1000 mL portions of diethyl ether in the manner
  7. customThe solid residue was dried under reduced pressure

出典と根拠

ORDレコード
ord-beb3490793244da9858492292b692270
出典データセット
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04975451

反応ノート

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