Dichloromethane → HCID 178496341、化合物

HRID 26445ノート

反応式

HRID 26445 の反応式
[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH2:9])[CH:5]=[C:4]([N:10]2[CH2:15][CH:14]=[CH:13][CH2:12][CH2:11]2)[N:3]=1.C(Cl)Cl.[CH3:19][O:20][CH2:21][CH2:22][O:23][C:24](Cl)=[O:25]>C(N(CC)CC)C>[N:10]1([C:4]2[N:3]=[C:2]([NH:1][C:24]([O:23][CH2:22][CH2:21][O:20][CH3:19])=[O:25])[N+:7]([O-:8])=[C:6]([NH:9][C:24]([O:23][CH2:22][CH2:21][O:20][CH3:19])=[O:25])[CH:5]=2)[CH2:11][CH:12]=[CH:13][CH2:14][CH2:15]1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 694002-Methoxyethyl chloroformateHCID 178507852HCID 178507852、化合物

生成物 1

HCID 178496341HCID 178496341、化合物

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

10 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]-pyrimidine-3-oxide are stirred at 5° C. in 150 ml. of methylene chloride and 30 ml. of triethylamine and treated with 20 ml. of chloroformic acid 2-methoxyethyl ester. The mixture is stirred at room temperature for 4 hours, then washed with water and extracted with methylene chloride. The organic phases are evaporated under reduced pressure and the residue is recrystallized from diethyl ether, there being obtained bis(2-methoxyethyl) 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 126°-128° C.

後処理

  1. washwashed with water
  2. extractionextracted with methylene chloride
  3. customThe organic phases are evaporated under reduced pressure
  4. customthe residue is recrystallized from diethyl ether, there

出典と根拠

ORDレコード
ord-e692b1acb2a5489b9ba6844e903683e5
出典データセット
uspto-grants-1979_04
特許番号
US04150132

反応ノート

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