Methoxydiphenylphosphine → 1,4-Bis(diphenylphosphinyl)phthalazine

HRID 224993

반응식

HRID 224993 반응식
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

참가 물질

4

반응물 2

HCID 77636MethoxydiphenylphosphineHCID 784901,4-Dichlorophthalazine

생성물 1

HCID 205394661,4-Bis(diphenylphosphinyl)phthalazine

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-2c0b36bd0b3b43708263e05158d1cd6f
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04234729

연결된 노트

불러오는 중…