Dichloromethane → HCID 178443805、化合物

HRID 46837

反応式

HRID 46837 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.[CH2:19]([O:27][C:28](Cl)=[O:29])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]>C(N(CC)CC)C>[N:10]1([C:4]2[N:3]=[C:2]([NH:1][C:28]([O:27][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[O:29])[N+:7]([O-:8])=[C:6]([NH:9][C:28]([O:27][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[O:29])[CH:5]=2)[CH2:11][CH:12]=[CH:13][CH2:14][CH2:15]1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 81956Carbonochloridic acid, octyl esterHCID 178507852HCID 178507852、化合物

生成物 1

HCID 178443805HCID 178443805、化合物

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

反応条件

温度
5 °C

実験手順

10 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide are suspended in 150 ml. of methylene chloride and 20 ml. of triethylamine. The suspension is cooled to 5° C. and 28 g. of chloroformic acid octyl ester are added dropwise while stirring. The mixture is cooled for 30 minutes and then stirred at room temperature for 1 hour. The mixture is extracted with methylene chloride, washed with water, dried over magnesium sulfate and evaporated under reduced pressure. The residue is recrystallized from methylene chloride/ethanol, there being obtained dioctyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 64° C.

後処理

  1. temperatureThe mixture is cooled for 30 minutes
  2. stirringstirred at room temperature for 1 hour
  3. extractionThe mixture is extracted with methylene chloride
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated under reduced pressure
  7. customThe residue is recrystallized from methylene chloride/ethanol, there

出典と根拠

ORDレコード
ord-0d5dd75d51ec4fc482b08a21147b6ca6
出典データセット
uspto-grants-1979_11
特許番号
US04175189

関連ノート

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