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

HRID 224994노트

반응식

HRID 224994 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 (shown by formula in Claim 11) 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-d8e70429cd784a9892318e10a17d9c3b
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04234729

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