Methoxydiphenylphosphine → HCID 20539463、化合物

HRID 224986

反応式

HRID 224986 の反応式
[C:1]([C:3]1[C:8]([C:9]#[N:10])=[N:7][C:6](Cl)=[C:5](Cl)[N:4]=1)#[N:2].[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:1]([C:3]1[C:8]([C:9]#[N:10])=[N:7][C:6]([P:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:20])=[C:5]([P:19]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:20])[N:4]=1)#[N:2]

参加物

4

反応物 2

HCID 77636MethoxydiphenylphosphineHCID 6078205,6-Dichloro-2,3-dicyanopyrazine

生成物 1

HCID 20539463HCID 20539463、化合物収率 65.9%

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

実験手順

To a stirred, refluxing solution of 5.00 g of 2,3-dicyano-5,6-dichloropyrazine in 100 ml of o-dichlorobenzene under nitrogen was added dropwise 10.00 g of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 4 hours and then allowed to stand overnight. The resulting solid was separated by filtration, washed with benzene and twice with hexane, recrystallized from 200 ml of o-dichlorobenzene, and dried at 80° C./0.1 mm (13 Pa) to give 8.08 g of 2,3-dicyano-5,6-bis(diphenylphosphinyl)pyrazine (shown by formula in Claim 5) as a white solid, decomposition beginning at 210° C. Anal. calcd for C30H20N4O2P2 : C, 67.93; H, 3.80; N, 10.56; P, 11.68. Found: C, 67.77; H, 3.92; N, 10.48; P, 11.18.

後処理

  1. additionAfter the addition
  2. temperaturethe mixture was refluxed for 4 hours
  3. customThe resulting solid was separated by filtration
  4. washwashed with benzene and twice with hexane
  5. customrecrystallized from 200 ml of o-dichlorobenzene
  6. customdried at 80° C./0.1 mm (13 Pa)

出典と根拠

ORDレコード
ord-eb641f0bc8eb40b4bce4f93b9d3f45aa
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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