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Potassium Carbonate → HCID 58911267, 화합물

HRID 1295809
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반응식

HRID 1295809 반응식
Br[CH2:2][CH2:3][CH2:4][C:5]([NH:7][C:8]1([N:11]2[CH:15]=[CH:14][N:13]=[CH:12]2)[CH2:10][CH2:9]1)=[O:6].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[N:11]1([C:8]2([N:7]3[CH2:2][CH2:3][CH2:4][C:5]3=[O:6])[CH2:10][CH2:9]2)[CH:15]=[CH:14][N:13]=[CH:12]1
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참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 58911254HCID 58911254, 화합물

생성물 1

HCID 58911267HCID 58911267, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In a 50 ml three necked flask fitted with a magnetic stirrer, under inert atmosphere, the crude 4-bromo-N-(l-imidazol-1-yl-cyclopropyl)-butyramide a18 (2.76 g), K2CO3 (1.26 g, 9.1 mmol) and KI (0.0075 g) in DMF (25 ml) are heated 3 h at 60° C., 17 h at 80° C., cooled down to room temperature and concentrated in vacuo. The reaction mixture is diluted with CH2Cl2, filtered and concentrated in vacuo to give the crude pyrrolidone (1.7 g). The residue is purified by chromatography on silicagel (CH2Cl2/MeOH/NH4OH: 95/4.5/05 (v/v/v)) to give, after treatment with HCl in ether (1 eq) and recrystallization in MeCN, 1-[l-(1H-imidazol-1-yl)cyclopropyl]pyrrolidin-2-one 23 (0.033 g, 7.5%) as an hydrochloride.

후처리

  1. concentrationconcentrated in vacuo
  2. additionThe reaction mixture is diluted with CH2Cl2
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-52b10fa113b44a2c9e20d5600c7ee7ba
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07244747B2

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