Diisopropylethylamine → 2-[(2,5-dichloro-4-pyrimidinyl)amino]-N-(2-hydroxyethyl)benzamide

HRID 1362852ノート

反応式

HRID 1362852 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([Cl:9])=[CH:4][N:3]=1.[NH2:10][C:11]1[CH:22]=[CH:21][CH:20]=[CH:19][C:12]=1[C:13]([NH:15][CH2:16][CH2:17][OH:18])=[O:14].C(N(C(C)C)CC)(C)C>C(O)(C)C>[Cl:1][C:2]1[N:7]=[C:6]([NH:10][C:11]2[CH:22]=[CH:21][CH:20]=[CH:19][C:12]=2[C:13]([NH:15][CH2:16][CH2:17][OH:18])=[O:14])[C:5]([Cl:9])=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 2372592,4,5-TrichloropyrimidineHCID 30164842-Amino-N-(2-hydroxyethyl)benzamide

生成物 1

HCID 579742162-[(2,5-dichloro-4-pyrimidinyl)amino]-N-(2-hydroxyethyl)benzamide収率 90.3%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
0 °C

実験手順

A round-bottomed flask was charged with 2,4,5-trichloropyrimidine (1.3 g, 4.4 mmol), 2-amino-N-(2-hydroxyethyl)benzamide (838 mg, 4.65 mmol), di-isopropyl-ethylamine (925 μL, 5.31 mmol) and 15 mL isopropanol. The flask was fitted with a reflux condenser and the reaction was heated to reflux and stirred for 18 h. A white solid appeared in the reaction mixture. The reaction was cooled to 0° C. and filtered and solid was washed with ether to afford 2-[(2,5-dichloro-4-pyrimidinyl)amino]-N-(2-hydroxyethyl)benzamide (1.3 g, 89%):

後処理

  1. customThe flask was fitted with a reflux condenser
  2. temperaturethe reaction was heated
  3. temperatureto reflux
  4. filtrationfiltered
  5. washsolid was washed with ether

出典と根拠

ORDレコード
ord-6a0236597c374509b988102e18f0c1b9
出典データセット
uspto-grants-2011_02
特許番号
US07884098B2

反応ノート

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