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Water → Diethyl [4-(diphenylphosphanyl)phenyl]phosphonate

HRID 2392846
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HRID 2392846 반응식
[CH:1]1[CH:6]=[CH:5][C:4]([P-:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:3][CH:2]=1.[K+].F[C:16]1[CH:21]=[CH:20][C:19]([P:22](=[O:29])([O:26][CH2:27][CH3:28])[O:23][CH2:24][CH3:25])=[CH:18][CH:17]=1.O>C1COCC1.[S].[P]>[C:8]1([P:7]([C:4]2[CH:3]=[CH:2][CH:1]=[CH:6][CH:5]=2)[C:16]2[CH:21]=[CH:20][C:19]([P:22](=[O:29])([O:26][CH2:27][CH3:28])[O:23][CH2:24][CH3:25])=[CH:18][CH:17]=2)[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 11042360KPPh2HCID 13508438Diethyl (4-fluorophenyl)phosphonate

생성물 1

HCID 15243843Diethyl [4-(diphenylphosphanyl)phenyl]phosphonate수율 82%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 178527701
HCID 178527701, 화합물
용매

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온도
23 °C

실험 절차

25.8 ml (12.9 mmol) of potassium diphenylphosphide solution in THF (manufacturer: Aldrich) are added dropwise at -5° C. to a solution of 3.09 g (13.2 mmol) of diethyl 4-fluorophenylphosphonate, prepared as described in Phosphorus Sulfur 1980, 9(2), 197.202, in 20.0 ml of THF. After stirring for 19 hours at 23° C., the mixture is hydrolyzed by adding 20 ml of degassed water and stirring for 15 min. After extraction with ethyl acetate, and drying the organic phase over Na2SO4, the mixture is concentrated on a rotary evaporator. 4.20 g of diethyl 4-diphenylphosphinophenylphosphonate (82% of theory) are obtained in the form of a pale yellow oil.

후처리

  1. customprepared
  2. stirringstirring for 15 min
  3. extractionAfter extraction with ethyl acetate
  4. dry with materialdrying the organic phase over Na2SO4
  5. concentrationthe mixture is concentrated on a rotary evaporator

출처 및 근거

ORD 기록
ord-f11c0f8b8bcd4d368d938c8c3361d411
출처 데이터셋
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05801263

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