2-{6-Azido-5-(4-methylphenyl)pyrimidin-4-yloxy}ethanol → 2-{6-Amino-5-(4-methylphenyl)-pyrimidin-4-yloxy}ethanol

HRID 1082299

反応式

HRID 1082299 の反応式
[N:1]([C:4]1[N:9]=[CH:8][N:7]=[C:6]([O:10][CH2:11][CH2:12][OH:13])[C:5]=1[C:14]1[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=1)=[N+]=[N-]>[C].[Pd].C(O)C>[NH2:1][C:4]1[N:9]=[CH:8][N:7]=[C:6]([O:10][CH2:11][CH2:12][OH:13])[C:5]=1[C:14]1[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=1

参加物

4

反応物 1

HCID 118077902-{6-Azido-5-(4-methylphenyl)pyrimidin-4-yloxy}ethanol

生成物 1

HCID 111182972-{6-Amino-5-(4-methylphenyl)-pyrimidin-4-yloxy}ethanol収率 89.7%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

A mixture of 2-{6-azido-5-(4-methylphenyl)pyrimidin-4-yloxy}ethanol (19.6 g), 10% palladium-carbon (50% moist) (4.0 g) and ethanol (240 ml) is subjected to catalytic hydrogenation at room temperature under hydrogen atmosphere (1 atm) for one hour. The catalyst is removed by filtration, and the filtrate is concentrated under reduced pressure. The residue is recrystallized from ethyl acetate/n-hexane to give 2-{6-amino-5-(4-methylphenyl)pyrimidin-4-yloxy}ethanol (15.9 g).

後処理

  1. customis subjected to catalytic hydrogenation at room temperature under hydrogen atmosphere
  2. customfor one hour
  3. customThe catalyst is removed by filtration
  4. concentrationthe filtrate is concentrated under reduced pressure
  5. customThe residue is recrystallized from ethyl acetate/n-hexane

出典と根拠

ORDレコード
ord-938db4b6a7e84b90807c1255f7dfd655
出典データセット
uspto-grants-1996_12
特許番号
US05589478

関連ノート

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