HCID 15591933, 화합물 → HCID 15591934, 화합물

HRID 1248369노트

반응식

HRID 1248369 반응식
[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]

참가 물질

4

반응물 2

HCID 15591933HCID 15591933, 화합물HCID 86740153HCID 86740153, 화합물

생성물 1

HCID 15591934HCID 15591934, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-dfff6a95e9d64e34bc4449bdac0cffe5
출처 데이터셋
uspto-grants-1985_06
특허 번호
US04523945

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