Dichloromethane → HCID 178452819、化合物

HRID 26443

反応式

HRID 26443 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:23][C:24](Cl)=[O:25])[CH2:20][CH2:21][CH3:22]>C(N(CC)CC)C>[N:10]1([C:4]2[N:3]=[C:2]([NH:1][C:24]([O:23][CH2:19][CH2:20][CH2:21][CH3:22])=[O:25])[N+:7]([O-:8])=[C:6]([NH:9][C:24]([O:23][CH2:19][CH2:20][CH2:21][CH3:22])=[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 61140Butyl chloroformateHCID 178507852HCID 178507852、化合物

生成物 1

HCID 178452819HCID 178452819、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

20 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide are mixed with 250 ml. of methylene chloride and 35 ml. of triethylamine, stirred and cooled to 5° C. The mixture is treated with 45 ml. of chloroformic acid butyl ester and stirred at room temperature for 6 hours. The mixture obtained is washed with water, extracted with methylene chloride and evaporated under reduced pressure. The residue is recrystallized from ethanol, there being obtained dibutyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 131°-132° C.

後処理

  1. additionThe mixture is treated with 45 ml
  2. customThe mixture obtained
  3. washis washed with water
  4. extractionextracted with methylene chloride
  5. customevaporated under reduced pressure
  6. customThe residue is recrystallized from ethanol, there

出典と根拠

ORDレコード
ord-aaf95424dd714d558075c4f775f387bd
出典データセット
uspto-grants-1979_04
特許番号
US04150132

関連ノート

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