Lithium hydroxide, monohydrate → 3-(2-Flourobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylic acid

HRID 1094734노트

반응식

HRID 1094734 반응식
[F:1][C:2]1[CH:23]=[CH:22][CH:21]=[CH:20][C:3]=1[CH2:4][N:5]1[C:14](=[O:15])[C:13]2[C:8](=[CH:9][C:10]([C:16]([O:18]C)=[O:17])=[CH:11][CH:12]=2)[N:7]=[CH:6]1.O[Li].O>C1COCC1.CO.O>[F:1][C:2]1[CH:23]=[CH:22][CH:21]=[CH:20][C:3]=1[CH2:4][N:5]1[C:14](=[O:15])[C:13]2[C:8](=[CH:9][C:10]([C:16]([OH:18])=[O:17])=[CH:11][CH:12]=2)[N:7]=[CH:6]1

참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 59842874Methyl 3-(2-flourobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboylate

생성물 1

HCID 598428393-(2-Flourobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylic acid수율 98.4%

시약·촉매·용매 1

HCID 21892291Methanol tetrahydrofuran water용매

실험 절차

Methyl 3-(2-flourobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboylate 300 mg, 0.92 mmol) was dissolved In a mixture of THF-MeOH—H2O (10 mL-3 mL-3 mL) followed by the addition of LiOH—H2O (200 mg). The mixture was stirred at RT over night. The solvent evaporated and the residue was dissolved in 4 mL of water and then acidified with 2N HCl to pH˜3. The solid was filtered off dried to gave 270 mg 3-(2-flourobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylic acid in 75% yield.

후처리

  1. customThe solvent evaporated
  2. dissolutionthe residue was dissolved in 4 mL of water
  3. filtrationThe solid was filtered off
  4. customdried

출처 및 근거

ORD 기록
ord-0286bc2666874943930cf4510462f99f
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08133998B2

반응 노트

불러오는 중…