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1-Ethyl hexanedioate → 3,5-Dichlorobenzyl 4-(6-ethoxy-6-oxohexanamido)piperidine-1-carboxylate

HRID 1480378
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인쇄 미리보기

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HRID 1480378 반응식
[CH2:1]([O:3][C:4](=[O:12])[CH2:5][CH2:6][CH2:7][CH2:8][C:9]([OH:11])=O)[CH3:2].Cl.[NH2:14][CH:15]1[CH2:20][CH2:19][N:18]([C:21]([O:23][CH2:24][C:25]2[CH:30]=[C:29]([Cl:31])[CH:28]=[C:27]([Cl:32])[CH:26]=2)=[O:22])[CH2:17][CH2:16]1.CCN(C(C)C)C(C)C.C(P1(=O)OP(CCC)(=O)OP(CCC)(=O)O1)CC>CN(C=O)C.CCOC(C)=O>[CH2:1]([O:3][C:4](=[O:12])[CH2:5][CH2:6][CH2:7][CH2:8][C:9]([NH:14][CH:15]1[CH2:16][CH2:17][N:18]([C:21]([O:23][CH2:24][C:25]2[CH:30]=[C:29]([Cl:31])[CH:28]=[C:27]([Cl:32])[CH:26]=2)=[O:22])[CH2:19][CH2:20]1)=[O:11])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 122951-Ethyl hexanedioateHCID 81531DiisopropylethylamineHCID 111923Propylphosphonic anhydrideHCID 867226383,5-Dichlorobenzyl 4-aminopiperidine-1-carboxylate hydrochloride

생성물 1

HCID 867226333,5-Dichlorobenzyl 4-(6-ethoxy-6-oxohexanamido)piperidine-1-carboxylate

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
2회
HCID 8857Ethyl Acetate용매

실험 절차

To a suspension of adipic acid mono ethyl ester (154 mg, 0.883 mmol) and 3,5-dichlorobenzyl 4-aminopiperidine-1-carboxylate HCl salt (Example 9, step 2)(300 mg, 0.883 mmol) in DMF (2 mL) was added Huenig's base (0.771 mL, 4.42 mmol) and T3P® (50% in DMF) (1.031 mL, 1.767 mmol) and the mixture was stirred at RT for 4 hrs. The resulting mixture was diluted with EtOAc and washed with a saturated solution of sodium bicarbonate.

후처리

  1. washwashed with a saturated solution of sodium bicarbonate

출처 및 근거

ORD 기록
ord-280f74a28804438db08760003ab058e8
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09409895B2

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