2,4,6-Trichloropyrimidine → 2,4,6-Tris(diphenylphosphinyl)pyrimidine

HRID 1065628

反応式

HRID 1065628 の反応式
Cl[C:2]1[N:7]=[C:6](Cl)[CH:5]=[C:4](Cl)[N:3]=1.[C:10]1([P:16]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[O:17]C)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>ClC1C=CC=CC=1Cl>[C:10]1([P:16]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)([C:2]2[N:7]=[C:6]([P:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)([C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=3)=[O:17])[CH:5]=[C:4]([P:16]([C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=3)([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)=[O:17])[N:3]=2)=[O:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

4

反応物 2

HCID 773782,4,6-TrichloropyrimidineHCID 77636Methoxydiphenylphosphine

生成物 1

HCID 205394672,4,6-Tris(diphenylphosphinyl)pyrimidine収率 61.2%

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

実験手順

To a stirred, refluxing mixture of 5.00 g of 2,4,6-trichloropyrimidine in 100 ml of o-dichlorobenzene under nitrogen was added dropwise 26.00 g of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 6.5 hours and then allowed to stand overnight at room temperature. The next day a small amount of the solvent was removed by boiling, and the solution was allowed to stand again overnight. The next day the resulting solid was separated by filtration, washed twice with benzene and three times with hexane, recrystallized from 650 ml of toluene, and dried at 100° C./0.1 mm (13 Pa) to give 11.35 g of 2,4,6-tris(diphenylphosphinyl)pyrimidine as a white solid, mp 235°-236° C. Anal. Calcd for C40H31N2O3P3 : C, 70.59; H, 4.59; N, 4.12; P, 13.65. Found: C, 70.72; H, 4.90; N, 3.92; P, 13.61.

後処理

  1. temperatureTo a stirred, refluxing
  2. additionAfter the addition
  3. temperaturethe mixture was refluxed for 6.5 hours
  4. customThe next day a small amount of the solvent was removed
  5. waitto stand again overnight
  6. customThe next day the resulting solid was separated by filtration
  7. washwashed twice with benzene and three times with hexane
  8. customrecrystallized from 650 ml of toluene
  9. customdried at 100° C./0.1 mm (13 Pa)

出典と根拠

ORDレコード
ord-17abd14d508746ad9783afbb2a7a4c1b
出典データセット
uspto-grants-1982_05
特許番号
US04330461

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