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Triphenylphosphine → HCID 86744367, 화합물

HRID 1110405
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HRID 1110405 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

HCID 86744367HCID 86744367, 화합물수율 79.6%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-beb3490793244da9858492292b692270
출처 데이터셋
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04975451

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