4-Fluorobenzylamine → HCID 178429626, 화합물

HRID 23630

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HRID 23630 반응식
[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

참가 물질

4

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bc944c46c3124ec2806eac8d44ed2373
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06852731B2

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