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Hydrochloric Acid → 1-[1-(Ethoxycarbonyl)azepan-4-yl]-4-methoxypiperidine-4-carboxylic acid

HRID 714542
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HRID 714542 반응식
[CH3:1][O:2][C:3]1([C:21]([O:23]C)=[O:22])[CH2:8][CH2:7][N:6]([CH:9]2[CH2:15][CH2:14][CH2:13][N:12]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:11][CH2:10]2)[CH2:5][CH2:4]1.[Li+].[OH-].Cl>C1COCC1>[CH2:19]([O:18][C:16]([N:12]1[CH2:13][CH2:14][CH2:15][CH:9]([N:6]2[CH2:5][CH2:4][C:3]([O:2][CH3:1])([C:21]([OH:23])=[O:22])[CH2:8][CH2:7]2)[CH2:10][CH2:11]1)=[O:17])[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 89579395Ethyl 4-[4-methoxy-4-(methoxycarbonyl)piperidin-1-yl]azepane-1-carboxylate

생성물 1

HCID 895794691-[1-(Ethoxycarbonyl)azepan-4-yl]-4-methoxypiperidine-4-carboxylic acid수율 102.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl 4-[4-methoxy-4-(methoxycarbonyl)piperidin-1-yl]azepane-1-carboxylate (0.136 g, 0.39 mmol) was dissolved in THF (5 mL) at rt and 1M LiOH sol. (0.4 mL) was added. The reaction mixture was stirred at rt for 2 days. 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]-4-methoxypiperidine-4-carboxylic acid (0.131 g), Intermediate 8, as a yellow oil which was used directly without further purification.

후처리

  1. customthe solvents were removed in vacuo

출처 및 근거

ORD 기록
ord-a415d3e58e664121892e9d481b0f47a2
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09187451B2

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