4,6-Dichloro-2-(methylthio)pyrimidine → HCID 20539481, 화합물

HRID 1065630노트

반응식

HRID 1065630 반응식
[CH:1]1([P:7]([CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[O:8]C)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl[C:17]1[CH:22]=[C:21](Cl)[N:20]=[C:19]([S:24][CH3:25])[N:18]=1>ClC1C=CC=CC=1Cl>[CH:1]1([P:7]([CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)([C:17]2[CH:22]=[C:21]([P:7]([CH:10]3[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]3)([CH:1]3[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]3)=[O:8])[N:20]=[C:19]([S:24][CH3:25])[N:18]=2)=[O:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 805314,6-Dichloro-2-(methylthio)pyrimidineHCID 6931439Phosphinous acid, dicyclohexyl-, methyl ester

생성물 1

HCID 20539481HCID 20539481, 화합물수율 5.3%

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

실험 절차

A mixture of 2.50 g of methyl dicyclohexylphosphinite and 1.00 g of 4,6-dichloro-2-methylthiopyrimidine in 20 ml of o-dichlorobenzene was refluxed under nitrogen for 6.5 hours. Volatiles were removed from the mixture under vacuum, and the resulting oily residue was recrystallized twice from cyclohexane with decolorizing charcoal treatment and dried at 100° C./0.1 mm (13 Pa) to give 0.15 g of 4,6-bis(dicyclohexylphosphinyl)-2-methylthiopyrimidine as white crystals, mp 197°-198.5° C. Anal. Calcd for C29H48N2O2P2S: C, 63.25; H, 8.79; N, 5.07; S, 5.82. Found: C, 63.19; H, 8.81; N, 4.89; S, 6.04.

후처리

  1. temperaturewas refluxed under nitrogen for 6.5 hours
  2. customVolatiles were removed from the mixture under vacuum
  3. customthe resulting oily residue was recrystallized twice from cyclohexane with decolorizing charcoal treatment
  4. customdried at 100° C./0.1 mm (13 Pa)

출처 및 근거

ORD 기록
ord-704f4a33043543b18857934e58b7b5f5
출처 데이터셋
uspto-grants-1982_05
특허 번호
US04330461

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