4-Fluorobenzylamine → HCID 178429626、化合物

HRID 23630

反応式

HRID 23630 の反応式
[OH:1][C:2]1[C:7]([C:8]([O:10]CC)=O)=[CH:6][N:5]=[C:4]2[C:13]([CH3:18])=[C:14]([CH2:16][OH:17])[S:15][C:3]=12.[F:19][C:20]1[CH:27]=[CH:26][C:23]([CH2:24][NH2:25])=[CH:22][CH:21]=1>Cl>[F:19][C:20]1[CH:27]=[CH:26][C:23]([CH2:24][NH:25][C:8]([C:7]2[C:2]([OH:1])=[C:3]3[S:15][C:14]([CH2:16][OH:17])=[C:13]([CH3:18])[C:4]3=[N:5][CH:6]=2)=[O:10])=[CH:22][CH:21]=1

参加物

4

反応物 2

HCID 673264-FluorobenzylamineHCID 178469552HCID 178469552、化合物

生成物 1

HCID 178429626HCID 178429626、化合物収率 85.5%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
80 °C

実験手順

A suspension of 140 mg (0.52 mmol) ethyl 7-hydroxy-2-(hydroxymethyl)-3-methylthieno[3,2-b]pyridine-6-carboxylate in 1.28 mL (11.2 mmol) 4-fluorobenzylamine was heated to 80° C. for 24 hours. The mixture was then cooled to room temperature and added to 10 mL of 1N HCl and then cooled in the refrigerator for three hours. The resulting mixture was then filtered and the obtained solid was washed with 1N HCl several times (50 mL total volume) and dried in a vacuum oven at 60° C. over night to provide 154 mg of the title compound as a tan solid.

後処理

  1. temperatureThe mixture was then cooled to room temperature
  2. temperaturecooled in the refrigerator for three hours
  3. filtrationThe resulting mixture was then filtered
  4. washthe obtained solid was washed with 1N HCl several times (50 mL total volume)
  5. customdried in a vacuum oven at 60° C. over night

出典と根拠

ORDレコード
ord-bc944c46c3124ec2806eac8d44ed2373
出典データセット
uspto-grants-2005_02
特許番号
US06852731B2

関連ノート

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