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Triphenylphosphine → HCID 19789980, 화합물

HRID 1656023
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HRID 1656023 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[CH:10]=2)[CH:5]=[CH:4][C:3]=1[OH:16].[Cl:17][C:18]1[CH:25]=[CH:24][C:21]([CH2:22]O)=[CH:20][CH:19]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1>[Cl:17][C:18]1[CH:25]=[CH:24][C:21]([CH2:22][O:16][C:3]2[CH:4]=[CH:5][C:6]([O:8][C:9]3[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[CH:10]=3)=[CH:7][C:2]=2[Cl:1])=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11776TriphenylphosphineHCID 133974-Chlorobenzyl alcoholHCID 19789982HCID 19789982, 화합물

생성물 1

HCID 19789980HCID 19789980, 화합물수율 62%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 0.88 g of 2-chloro-4-(3-fluorophenoxy)phenol, 0.54 g of p-chlorobenzyl alcohol, 1.01 g of triphenylphosphine, 0.65 g of diethylazadicarboxylate and 90 ml of tetrahydrofuran was stirred at room temperature. After 48 hours, the reaction mixture was concentrated, and 50 ml of diethyl ether was added thereto. The precipitates were removed by filtration, and the filtrate was concentrated. The residue was subjected to silica gel chromatography to give 0.83 g of 4-chloro-1-[2-chloro-4-(3-fluorophenoxy)phenoxy]methylbenzene. Yield, 62%. m.p., 47.3° C.

후처리

  1. concentrationthe reaction mixture was concentrated
  2. addition50 ml of diethyl ether was added
  3. customThe precipitates were removed by filtration
  4. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-cab897fe987d463181f4d0671b04d049
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05252610

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