Hydrochloric Acid → 5-[(3-{[(1,1-Dimethylethyl)oxy]carbonyl}-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)oxy]-2-pyrazinecarboxylic acid

HRID 645796노트

반응식

HRID 645796 반응식
[OH-].[Na+].C[O:4][C:5]([C:7]1[N:8]=[CH:9][C:10]([O:13][C:14]2[CH:31]=[CH:30][C:17]3[CH2:18][CH2:19][N:20]([C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])[CH2:21][CH2:22][C:16]=3[CH:15]=2)=[N:11][CH:12]=1)=[O:6].Cl.O>CC(C)=O>[CH3:29][C:26]([O:25][C:23]([N:20]1[CH2:19][CH2:18][C:17]2[CH:30]=[CH:31][C:14]([O:13][C:10]3[N:11]=[CH:12][C:7]([C:5]([OH:6])=[O:4])=[N:8][CH:9]=3)=[CH:15][C:16]=2[CH2:22][CH2:21]1)=[O:24])([CH3:27])[CH3:28]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 589845771,1-Dimethylethyl 7-({5-[(methyloxy)carbonyl]-2-pyrazinyl}oxy)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate

생성물 1

HCID 574376215-[(3-{[(1,1-Dimethylethyl)oxy]carbonyl}-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)oxy]-2-pyrazinecarboxylic acid수율 96.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

2M Sodium hydroxide solution (110 ml) was added to a solution of 1,1-dimethylethyl 7-({5-[(methyloxy)carbonyl]-2-pyrazinyl}oxy)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (D49, Step 1) (29.38 g, 73.6 mmol) in acetone (480 ml) and the resulting mixture was stirred at room temperature for 25 minutes. The mixture was acidified with 2M hydrochloric acid and then poured into water (2 L). The resulting white solid was collected by filtration, washed with water and dissolved in ethyl acetate (1 L). This solution was dried under sodium sulfate and evaporated in vacuo to give the title compound (27.3 g); MS (ES+) m/e 384 [M−H]+.

후처리

  1. filtrationThe resulting white solid was collected by filtration
  2. washwashed with water
  3. dissolutiondissolved in ethyl acetate (1 L)
  4. customThis solution was dried under sodium sulfate
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-46947d5a9f2a46c384ae0c04ba771b56
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07704994B2

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