1,2-Dichlorobenzene → HCID 20539464、化合物

HRID 224990

反応式

HRID 224990 の反応式
Cl[C:2]1[CH:7]=[C:6](Cl)[N:5]=[CH:4][N:3]=1.Cl[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1Cl.[C:17]1([P:23]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[O:24]C)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>CCCCCC>[C:10]1([P:23]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)([C:2]2[CH:7]=[C:6]([P:23]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[O:24])[N:5]=[CH:4][N:3]=2)=[O:24])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 72391,2-DichlorobenzeneHCID 709434,6-DichloropyrimidineHCID 77636Methoxydiphenylphosphine

生成物 1

HCID 20539464HCID 20539464、化合物

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

To a stirred, refluxing mixture of 5.00 g 4,6-dichloropyrimidine in 100 of o-dichlorobenzene under nitrogen was added dropwise 17.00 g of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 6.5 hours and then allowed to cool. The cooled mixture was added to 750 ml of n-hexane, and the white solid that formed was separated by filtration, washed with n-hexane, recrystallized from 150 ml of toluene, and dried at 100° C./0.1 mm (13 Pa) to give 13.64 g of 4,6-bis(diphenylphosphinyl)pyrimidine (shown by formula in Claim 9) as cream-colored crystals, mp 213°-215° C. Anal. Calcd for C28H22N2O2P2 : C, 70.00; H, 4.62; N, 5.83; P, 12.89. Found: C, 69.80; H, 4.65; N, 5.65; P, 12.89.

後処理

  1. temperatureTo a stirred, refluxing
  2. additionAfter the addition
  3. temperaturethe mixture was refluxed for 6.5 hours
  4. temperatureto cool
  5. customthe white solid that formed
  6. customwas separated by filtration
  7. washwashed with n-hexane
  8. customrecrystallized from 150 ml of toluene
  9. customdried at 100° C./0.1 mm (13 Pa)

出典と根拠

ORDレコード
ord-a8ed9376caff466cadcc70b5dbf726ef
出典データセット
uspto-grants-1980_11
特許番号
US04234729

関連ノート

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