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Diisopropylethylamine → N-[4-bromo-3-(methyloxy)phenyl]-2-{[(3S)-1-(cyclopropylcarbonyl)-3-pyrrolidinyl]acetyl}hydrazinecarboxamide

HRID 2405354
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HRID 2405354 반응식
Cl[C:2](Cl)([O:4]C(=O)OC(Cl)(Cl)Cl)Cl.[CH3:13][O:14][C:15]1[CH:16]=[C:17]([CH:19]=[CH:20][C:21]=1[Br:22])[NH2:18].CCN(C(C)C)C(C)C.[CH:32]1([C:35]([N:37]2[CH2:41][CH2:40][C@@H:39]([CH2:42][C:43]([NH:45][NH2:46])=[O:44])[CH2:38]2)=[O:36])[CH2:34][CH2:33]1>ClCCl>[Br:22][C:21]1[CH:20]=[CH:19][C:17]([NH:18][C:2]([NH:46][NH:45][C:43](=[O:44])[CH2:42][C@@H:39]2[CH2:40][CH2:41][N:37]([C:35]([CH:32]3[CH2:34][CH2:33]3)=[O:36])[CH2:38]2)=[O:4])=[CH:16][C:15]=1[O:14][CH3:13]
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참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 94429TriphosgeneHCID 70182544-Bromo-3-methoxyanilineHCID 673540782-[(3S)-1-(cyclopropylcarbonyl)-3-pyrrolidinyl]acetohydrazide

생성물 1

HCID 71087558N-[4-bromo-3-(methyloxy)phenyl]-2-{[(3S)-1-(cyclopropylcarbonyl)-3-pyrrolidinyl]acetyl}hydrazinecarboxamide

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
3회

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온도
-78 °C

실험 절차

To a round bottom flask was added triphosgene (0.514 g, 1.732 mmol) and dichloromethane (30 mL) under nitrogen, and the solution was cooled to −78° C. In a separate vial, 3-methoxy 4-bromoaniline (1 g, 4.95 mmol) was dissolved in dichloromethane (20 mL) and Hunig's base (1.753 mL, 9.90 mmol) was added. This solution was slowly added to the cooled solution and then the reaction was allowed to warm to room temperature. Analysis by LCMS indicated desired intermediate formation. The reaction was cooled again to −78° C. and 2-[(3S)-1-(cyclopropylcarbonyl)-3-pyrrolidinyl]acetohydrazide (0.575 g, 2.72 mmol) in dichloromethane (5 mL) was added slowly. The reaction was allowed to warm to room temperature and analysis by LCMS indicated desired product formation. The reaction was poured into a reparatory funnel and partitioned with saturated aq sodium bicarbonate. The aqueous layer was extracted with dichloromethane (3×) and the combined organic layers were dried over sodium sulfate, filtered, and concentrated in vacuo to an oil. The residue was purified by silica gel chromatography (0-40% isopropanol/ethyl acetate). The desired product fractions were combined and concentrated in vacuo to afford the title product as a tan solid (500 mg, 42%). MS(ES)+ m/e 439.0, 441.1 M+H]+.

후처리

  1. additionThis solution was slowly added to the cooled solution
  2. temperatureto warm to room temperature
  3. temperatureThe reaction was cooled again to −78° C.
  4. temperatureto warm to room temperature

출처 및 근거

ORD 기록
ord-dc56ef5e55694c569bd6a5e2a705b5cf
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08802864B2

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