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Triethylamine → carbonic acid 4-(2,5-dimethyl-phenyl)-2-(1-methoxy-piperidin-4-ylmethyl)-5-oxo-2,5-dihydro-1H-pyrrol-3-yl ester ethyl ester

HRID 1844664
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HRID 1844664 반응식
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[CH3:7][C:8]1[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][C:9]=1[C:15]1[C:16](=[O:30])[NH:17][CH:18]([CH2:21][CH:22]2[CH2:27][CH2:26][N:25]([O:28][CH3:29])[CH2:24][CH2:23]2)[C:19]=1[OH:20].CCN(CC)CC>CN(C1C=CN=CC=1)C.C1COCC1>[CH2:5]([O:4][C:2](=[O:3])[O:20][C:19]1[CH:18]([CH2:21][CH:22]2[CH2:23][CH2:24][N:25]([O:28][CH3:29])[CH2:26][CH2:27]2)[NH:17][C:16](=[O:30])[C:15]=1[C:9]1[CH:10]=[C:11]([CH3:14])[CH:12]=[CH:13][C:8]=1[CH3:7])[CH3:6]
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 682992393-(2,5-Dimethyl-phenyl)-4-hydroxy-5-(1-methoxy-piperidin-4-ylmethyl)-1,5-dihydro-pyrrol-2-one

생성물 1

HCID 68299269carbonic acid 4-(2,5-dimethyl-phenyl)-2-(1-methoxy-piperidin-4-ylmethyl)-5-oxo-2,5-dihydro-1H-pyrrol-3-yl ester ethyl ester

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine
촉매
HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl chloroformate (72 mg, 0.67 mmol) was added dropwise to a solution of 3-(2,5-dimethyl-phenyl)-4-hydroxy-5-(1-methoxy-piperidin-4-ylmethyl)-1,5-dihydro-pyrrol-2-one (220 mg, 0.67 mmol), Et3N (94 mg, 0.9 mmol) and DMAP (30 mg, 0.25 mmol) in 10 ml of THF at room temperature. The mixture was stirred for 30 min and concentrated to dryness in vacuo. The residue was purified by column chromatography on silica gel. Yield: 150 mg of carbonic acid 4-(2,5-dimethyl-phenyl)-2-(1-methoxy-piperidin-4-ylmethyl)-5-oxo-2,5-dihydro-1H-pyrrol-3-yl ester ethyl ester (title compound P1.1) as a gum.

후처리

  1. concentrationconcentrated to dryness in vacuo
  2. customThe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-01fd87e9a9df45fa831fe88d62545864
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946453B2

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