Phosphorodichloridous acid, methyl ester → Di[p-(3-phenylpropyl)phenyl]chlorophosphine

HRID 1955942노트

반응식

HRID 1955942 반응식
[C:1]1([CH2:7][CH2:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([Li])=[CH:12][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO[P:19]([Cl:21])Cl>>[C:1]1([CH2:7][CH2:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([P:19]([C:13]3[CH:14]=[CH:15][C:10]([CH2:9][CH2:8][CH2:7][C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)=[CH:11][CH:12]=3)[Cl:21])=[CH:12][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

3

반응물 2

HCID 76768Phosphorodichloridous acid, methyl esterHCID 178506705HCID 178506705, 화합물

생성물 1

HCID 11113246Di[p-(3-phenylpropyl)phenyl]chlorophosphine수율 90%

실험 절차

p-(3-phenylpropyl)phenyllithium (8.1 g, 40 mmol) in 150 ml solvent (Et2O/THF 1/1) was added dropwise to CH3OPCl2 (2.66 g, 20 mmol) in 70 ml solvent (Et2O/THF 1/1) at -70° C. The addition was completed in 2 h. The reaction mixture was stirred overnight at room temperature and then brought to reflux for 2 h. The precipitate was filtered and the solvent of the solution was removed by applying vacuum. PCl3 (15 ml) was added to the resulting viscous oil and stirred for 24 h. Then the mixture was kept at 70° C. and 1 mm Hg for 2 h to remove excess PCl3 and byproduct. The product, di[p-(3-phenylpropyl)phenyl]chlorophosphine, was obtained as a pale yellow viscous oil with 90% yield. The product was characterized by 31P NMR. 83.6.

후처리

  1. additionThe addition
  2. temperatureto reflux for 2 h
  3. filtrationThe precipitate was filtered
  4. customthe solvent of the solution was removed
  5. additionPCl3 (15 ml) was added to the resulting viscous oil
  6. stirringstirred for 24 h
  7. customwas kept at 70° C.
  8. custom1 mm Hg for 2 h to remove excess PCl3 and byproduct

출처 및 근거

ORD 기록
ord-372abff4445144ac8fc6676e4cf39aaf
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05777087

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