HCID 13039363、化合物 → HCID 70504731、化合物

HRID 1395438ノート

反応式

HRID 1395438 の反応式
[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]

参加物

4

反応物 2

HCID 13039363HCID 13039363、化合物HCID 178479487HCID 178479487、化合物

生成物 1

HCID 70504731HCID 70504731、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-884d0a112cbe4855a320215842a333c4
出典データセット
uspto-grants-1980_05
特許番号
US04203985

反応ノート

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