Methoxydiphenylphosphine → 1,4-Bis(diphenylphosphinyl)phthalazine

HRID 224993

反応式

HRID 224993 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5](Cl)=[N:4][N:3]=1.[C:13]1([P:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[O:20]C)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>ClC1C=CC=CC=1Cl>[C:13]1([P:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)([C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]([P:19]([C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=3)([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[O:20])=[N:4][N:3]=2)=[O:20])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

4

反応物 2

HCID 77636MethoxydiphenylphosphineHCID 784901,4-Dichlorophthalazine

生成物 1

HCID 205394661,4-Bis(diphenylphosphinyl)phthalazine

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 1,4-dichlorophthalazine in 50 ml of o-dichlorobenzene under nitrogen was added dropwise 15.00 of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 6 hours and then allowed to stand at room temperature for 13 days. The resulting solid was separated by filtration, washed with benzene and with hexane, recrystallized from 125 ml of toluene with decolorizing charcoal treatment, and dried at 100° C./0.1 mm (13 Pa) to give 6.41 g of 1,4-bis(diphenylphosphinyl)phthalazine (shown by formula in Claim 13) as a light-yellow solid, mp 225°-228.5° C. Anal. Calcd C32H24N2O2P2 : C, 72.45; H, 4.56; N, 5.28; P, 11.68. Found: C, 72.49; H, 4.62; N, 5.36; P, 11.95.

後処理

  1. temperatureTo a stirred, refluxing
  2. additionAfter the addition
  3. temperaturethe mixture was refluxed for 6 hours
  4. customThe resulting solid was separated by filtration
  5. washwashed with benzene and with hexane
  6. customrecrystallized from 125 ml of toluene with decolorizing charcoal treatment
  7. customdried at 100° C./0.1 mm (13 Pa)

出典と根拠

ORDレコード
ord-2c0b36bd0b3b43708263e05158d1cd6f
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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