Lithium Hydroxide → 3-bromo-7-[(tert-butoxy)carbonyl]-5H,6H,7H,8H-imidazo[1,5-a]pyrazine-1-carboxylic acid

HRID 1971074노트

반응식

HRID 1971074 반응식
[Br:1][C:2]1[N:6]2[CH2:7][CH2:8][N:9]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:10][C:5]2=[C:4]([C:18]([O:20]C)=[O:19])[N:3]=1.[Li+].[OH-]>CO.O>[Br:1][C:2]1[N:6]2[CH2:7][CH2:8][N:9]([C:11]([O:13][C:14]([CH3:15])([CH3:16])[CH3:17])=[O:12])[CH2:10][C:5]2=[C:4]([C:18]([OH:20])=[O:19])[N:3]=1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 576351407-(tert-Butyl) 1-methyl 3-bromo-5,6-dihydroimidazo[1,5-a]pyrazine-1,7(8H)-dicarboxylate

생성물 1

HCID 576354283-bromo-7-[(tert-butoxy)carbonyl]-5H,6H,7H,8H-imidazo[1,5-a]pyrazine-1-carboxylic acid수율 76%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

The product Intermediate 1H (0.85 g, 2.36 mmol) was dissolved in methanol (50 mL) and LiOH (0.79 g, 18.88 mmol) in water (10 mL) was added. The resulting solution was stirred at 50° C. overnight. The reaction mixture was concentrated, cooled on ice and brought to pH 3 using 1N HCl. The resulting white precipitate was filtered, washed with water and air dried to give the desired acid Intermediate 1I as a white solid (0.62 g, 76%).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. temperaturecooled on ice
  3. filtrationThe resulting white precipitate was filtered
  4. washwashed with water and air
  5. customdried

출처 및 근거

ORD 기록
ord-4fa68796a5114239b67705047b1b1158
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08431565B2

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