HCID 15591933、化合物 → HCID 15591934、化合物

HRID 1248369ノート

反応式

HRID 1248369 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4]([NH:9][CH2:10][CH:11]2[CH2:13][C:12]2([Cl:15])[Cl:14])[N:3]=1.[C:16](O)(=[O:18])C.C(OC=O)=O>C(#N)C>[CH:16]([NH:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4]([NH:9][CH2:10][CH:11]2[CH2:13][C:12]2([Cl:14])[Cl:15])[N:3]=1)=[O:18]

参加物

4

反応物 2

HCID 15591933HCID 15591933、化合物HCID 86740153HCID 86740153、化合物

生成物 1

HCID 15591934HCID 15591934、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

A solution of 2.7 g (0.01 mol) of 2-amino-4-chloro-6-{[(2,2-dichloro-cyclopropyl)methyl]amino}pyrimidine in 300 ml of acetonitrile was added dropwise, while stirring, at room temperature over a period of 15 minutes to a solution of 0.9 gm (0.012 mol) of acetic acid-formic acid anhydride in 5 ml of acetonitrile. After stirring the mixture for about 30 hours at room temperature the solvent was distilled off in vacuo, and the residue was treated twice by dissolving it in about 30 ml of toluene and then distilling the toluene off again. The raw product was purified by column chromatography (150 gm silica gel; eluant: Diisopropyl ether/ethyl acetate 9:1), yielding the title compound as white crystals.

後処理

  1. distillationwas distilled off in vacuo
  2. additionthe residue was treated twice
  3. dissolutionby dissolving it in about 30 ml of toluene
  4. distillationdistilling the toluene off again
  5. customThe raw product was purified by column chromatography (150 gm silica gel; eluant: Diisopropyl ether/ethyl acetate 9:1)

出典と根拠

ORDレコード
ord-dfff6a95e9d64e34bc4449bdac0cffe5
出典データセット
uspto-grants-1985_06
特許番号
US04523945

反応ノート

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