Hydrazine hydrate (1:1) → {6-[2-(3-Fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-5-propyl-pyrimidin-4-yl}-hydrazine

HRID 916650ノート

反応式

HRID 916650 の反応式
Cl[C:2]1[C:7]([CH2:8][CH2:9][CH3:10])=[C:6]([CH2:11][N:12]2[CH:16]=[CH:15][N:14]=[C:13]2[C:17]2[C:22]([F:23])=[CH:21][CH:20]=[CH:19][N:18]=2)[N:5]=[CH:4][N:3]=1.C(C1C(Cl)=NC=NC=1CBr)CC.FC1C(C2NC=CN=2)=NC=CC=1.O.[NH2:49][NH2:50]>CCO>[F:23][C:22]1[C:17]([C:13]2[N:12]([CH2:11][C:6]3[N:5]=[CH:4][N:3]=[C:2]([NH:49][NH2:50])[C:7]=3[CH2:8][CH2:9][CH3:10])[CH:16]=[CH:15][N:14]=2)=[N:18][CH:19]=[CH:20][CH:21]=1

参加物

6

反応物 4

HCID 24654Hydrazine hydrate (1:1)HCID 100423524-Chloro-6-{[2-(3-fluoro-2-pyridinyl)-1H-imidazol-1-yl]methyl}-5-propylpyrimidineHCID 223131604-Bromomethyl-5-propyl-6-chloro-pyrimidineHCID 223131643-Fluoro-2-(1H-imidazol-2-yl)pyridine

生成物 1

HCID 57503304{6-[2-(3-Fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-5-propyl-pyrimidin-4-yl}-hydrazine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

A mixture of 4-chloro-6-[2-(3-fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-5-propyl-pyrimidine (prepared from 5-propyl-6-bromomethyl-4-chloro-pyrimidine and 3-fluoro-2-(1H-imidazol-2-yl)-pyridine essentially as described in Example 1) (2.5 g, 7.5 mmol) and hydrazine monohydrate (1.37 g, 27.4 mmol) in EtOH (15 mL) is heated in a sealed tube at 70° C. overnight. The solvent is removed in vacuo and the residue is triturated with ethyl acetate and ethyl ether. Filtration gives a white solid (131) which is used in the next step without further purification.

後処理

  1. customThe solvent is removed in vacuo
  2. customthe residue is triturated with ethyl acetate and ethyl ether
  3. filtrationFiltration

出典と根拠

ORDレコード
ord-6e3a17f9a35e4b42909332e337c702c5
出典データセット
uspto-grants-2007_09
特許番号
US07271170B2

反応ノート

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