Hexane → HCID 20539492、化合物

HRID 224988

反応式

HRID 224988 の反応式
Cl[C:2]1[CH:7]=[C:6](Cl)[N:5]=[C:4]([S:9][CH3:10])[N:3]=1.[C:11]1([P:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[O:18]C)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[CH3:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31]>ClC1C=CC=CC=1Cl>[C:11]1([P:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)([C:2]2[CH:7]=[C:6]([P:17]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)([C:28]3[CH:27]=[CH:26][CH:31]=[CH:30][CH:29]=3)=[O:18])[N:5]=[C:4]([S:9][CH3:10])[N:3]=2)=[O:18])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 8058HexaneHCID 77636MethoxydiphenylphosphineHCID 805314,6-Dichloro-2-(methylthio)pyrimidine

生成物 1

HCID 20539492HCID 20539492、化合物

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 4,6-dichloro-2-methylthiopyrimidine in 150 ml of o-dichlorobenzene under nitrogen was added dropwise 15.00 g of methyl diphenylphosphinite over 35 minutes. The mixture was refluxed for 5.5 hours after the addition was completed and then allowed to cool, at which time it was added to 850 ml of n-hexane. The resulting solid was separated by filtration, washed with n-hexane, and recrystallized from 100 ml of ethanol to give 11.00 g of 4,6-bis(diphenylphosphinyl)-2-methylthiopyrimidine (shown by formula in Claim 8) as white crystals, mp 221°-222° C. Anal. Calcd for C29H24N2O2P2S: C, 66.15; H, 4.59; N, 5.32. Found: C, 65.59; 65.59; H, 4.54, 4.75; N, 5.04, 5.01.

後処理

  1. temperatureThe mixture was refluxed for 5.5 hours
  2. additionafter the addition
  3. temperatureto cool, at which time it
  4. customThe resulting solid was separated by filtration
  5. washwashed with n-hexane
  6. customrecrystallized from 100 ml of ethanol

出典と根拠

ORDレコード
ord-dd40434377704e66bcdb9580ce352c92
出典データセット
uspto-grants-1980_11
特許番号
US04234729

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