Hydrochloric Acid → 1-(1-(Ethoxycarbonyl)azepan-4-yl)piperidine-4-carboxylic acid

HRID 714528노트

반응식

HRID 714528 반응식
C([O:3][C:4]([CH:6]1[CH2:11][CH2:10][N:9]([CH:12]2[CH2:18][CH2:17][CH2:16][N:15]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:14][CH2:13]2)[CH2:8][CH2:7]1)=[O:5])C.[Li+].[OH-].Cl>C1COCC1>[CH2:22]([O:21][C:19]([N:15]1[CH2:16][CH2:17][CH2:18][CH:12]([N:9]2[CH2:10][CH2:11][CH:6]([C:4]([OH:5])=[O:3])[CH2:7][CH2:8]2)[CH2:13][CH2:14]1)=[O:20])[CH3:23]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 89579373Ethyl 4-[4-(ethoxycarbonyl)piperidin-1-yl]azepane-1-carboxylate

생성물 1

HCID 895794231-(1-(Ethoxycarbonyl)azepan-4-yl)piperidine-4-carboxylic acid수율 147.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl 4-[4-(ethoxycarbonyl)piperidin-1-yl]azepane-1-carboxylate (1.10 g, 3.4 mmol) was dissolved in THF (60 mL) at rt and 1M LiOH sol. (10 mL) was added. The reaction mixture was stirred at rt for 5 d. The pH was carefully adjusted to pH 6 by addition of concentrated hydrochloric acid, the solvents were removed in vacuo, to give 1-(1-(ethoxycarbonyl)azepan-4-yl)piperidine-4-carboxylic acid (1.5 g) as a viscous pale yellow oil, Intermediate 2, which was used crude in subsequent reactions.

후처리

  1. customthe solvents were removed in vacuo

출처 및 근거

ORD 기록
ord-d3ea529f161f49c495790f3fb507d7b5
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187451B2

반응 노트

불러오는 중…