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

HRID 714530ノート

反応式

HRID 714530 の反応式
[F:1][C:2]1([C:20]([O:22]CC)=[O:21])[CH2:7][CH2:6][N:5]([CH:8]2[CH2:14][CH2:13][CH2:12][N:11]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:10][CH2:9]2)[CH2:4][CH2:3]1.[Li+].[OH-].Cl>C1COCC1>[CH2:18]([O:17][C:15]([N:11]1[CH2:12][CH2:13][CH2:14][CH:8]([N:5]2[CH2:4][CH2:3][C:2]([F:1])([C:20]([OH:22])=[O:21])[CH2:7][CH2:6]2)[CH2:9][CH2:10]1)=[O:16])[CH3:19]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 89579328Ethyl 4-[4-fluoro-4-(ethoxycarbonyl)piperidin-1-yl]azepane-1-carboxylate

生成物 1

HCID 895795461-[1-(Ethoxycarbonyl)azepan-4-yl]-4-fluoropiperidine-4-carboxylic acid収率 148.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Ethyl 4-[4-fluoro-4-(ethoxycarbonyl)piperidin-1-yl]azepane-1-carboxylate (2.26 g, 6.85 mmol) was dissolved in THF (60 mL) at rt and 1M LiOH sol. (6.5 mL) was added. The reaction mixture was stirred at rt overnight. 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-fluoropiperidine-4-carboxylic acid (3.21 g) as a white waxy solid, Intermediate 3, which was used crude in subsequent reactions.

後処理

  1. customthe solvents were removed in vacuo

出典と根拠

ORDレコード
ord-8e3a20a5d77c4f428cd3c62235d346d6
出典データセット
uspto-grants-2015_11
特許番号
US09187451B2

反応ノート

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