HCID 13039363, 화합물 → HCID 70504731, 화합물

HRID 2049547노트

반응식

HRID 2049547 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]1[CH:14]=[N:13][C:12]([NH:15][CH3:16])=[N:11][C:10]1=[O:17].Cl.C(NC(N)=O)(=N)N>CO>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]1[CH:14]=[N:13][CH:12]([NH:15][CH3:16])[NH:11][C:10]1=[O:17]

참가 물질

4

반응물 2

HCID 13039363HCID 13039363, 화합물HCID 178479487HCID 178479487, 화합물

생성물 1

HCID 70504731HCID 70504731, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The reaction mixture was stirred for 1.5 hours after which an aliquot of the reaction product which had been dissolved in MeOH showed there to be one major spot with Rf equal to that of 1-(2-chloro-6-methylphenyl)-4-methylamino-1,2-dihydro-1,3,5-triazin-2-one and two minor spots of very small Rf, one at the origin and one of the same Rf as the starting material amidinourea hydrochloride. The reaction mixture was allowed to stir an additional 0.5 hour and the solid was filtered to yield 1-(2-chloro-6-methylphenyl)-4-methylaminodihydro-1,3,5-triazin-2-one, (EtOAc:MeOH; 9:1). It has the same two impurities as the crude reaction mixture. 7.7 g of the crude mixture was recrystallized from absolute EtOH; melting point 257.5°-258.5° C.

후처리

  1. stirringto stir an additional 0.5 hour
  2. filtrationthe solid was filtered

출처 및 근거

ORD 기록
ord-7a8db1bfb78642989c7a075657b6b99b
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04198409

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