Hexane → HCID 20539492, 화합물

HRID 224988

반응식

HRID 224988 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 20539492HCID 20539492, 화합물

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dd40434377704e66bcdb9580ce352c92
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04234729

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