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Hydrochloric Acid → 6-((1-(((3,5-Dichlorobenzyl)oxy)carbonyl)piperidin-4-yl)amino)-6-oxohexanoic acid

HRID 1480379
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HRID 1480379 반응식
C([O:3][C:4](=[O:30])[CH2:5][CH2:6][CH2:7][CH2:8][C:9]([NH:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]([O:20][CH2:21][C:22]2[CH:27]=[C:26]([Cl:28])[CH:25]=[C:24]([Cl:29])[CH:23]=2)=[O:19])[CH2:14][CH2:13]1)=[O:10])C.O[Li].O.Cl>C1COCC1.O.CCOC(C)=O>[Cl:28][C:26]1[CH:27]=[C:22]([CH:23]=[C:24]([Cl:29])[CH:25]=1)[CH2:21][O:20][C:18]([N:15]1[CH2:16][CH2:17][CH:12]([NH:11][C:9](=[O:10])[CH2:8][CH2:7][CH2:6][CH2:5][C:4]([OH:30])=[O:3])[CH2:13][CH2:14]1)=[O:19]
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참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 867226333,5-Dichlorobenzyl 4-(6-ethoxy-6-oxohexanamido)piperidine-1-carboxylate

생성물 1

HCID 867226326-((1-(((3,5-Dichlorobenzyl)oxy)carbonyl)piperidin-4-yl)amino)-6-oxohexanoic acid

시약·촉매·용매 3

HCID 962Water용매2회
HCID 8028
Tetrahydrofuran
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a suspension of 3,5-dichlorobenzyl 4-(6-ethoxy-6-oxohexanamido)piperidine-1-carboxylate (step 1) (130 mg, 0.283 mmol) in THF (3 mL)/water (1 mL) was added LiOH.H2O (26.1 mg, 0.623 mmol) and the reaction mixture stirred at RT for 3 hrs. The resulting mixture was diluted with water and EtOAc and the aqueous portion acidified with 0.1 M HCl solution (pH 5-6). The resulting precipitate was collected by filtration and washed with water to afford the title product;

후처리

  1. filtrationThe resulting precipitate was collected by filtration
  2. washwashed with water

출처 및 근거

ORD 기록
ord-027b68c76d3349f5860a911c93bb1cfd
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09409895B2

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