Methanol → HCID 86648961, 화합물

HRID 449921노트

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HRID 449921 반응식
[Cl:1][C:2]1[CH:22]=[C:21]([CH:23]=C)[CH:20]=[C:19]([Cl:25])[C:3]=1[C:4]([NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([NH:13][C:14]([CH:16]2[CH2:18][CH2:17]2)=[O:15])[CH:8]=1)=[O:5].C[OH:27]>C(Cl)Cl>[Cl:25][C:19]1[CH:20]=[C:21]([CH:23]=[O:27])[CH:22]=[C:2]([Cl:1])[C:3]=1[C:4]([NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([NH:13][C:14]([CH:16]2[CH2:17][CH2:18]2)=[O:15])[CH:8]=1)=[O:5]

참가 물질

4

반응물 2

HCID 887MethanolHCID 671286562,6-dichloro-N-(2-(cyclopropanecarboxamido)pyridin-4-yl)-4-vinylbenzamide

생성물 1

HCID 86648961HCID 86648961, 화합물수율 86%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
-78 °C

실험 절차

2,6-dichloro-N-(2-(cyclopropanecarboxamido)pyridin-4-yl)-4-vinylbenzamide (750 mg, 1.99 mmol) was dissolved in a solution of MeOH (14 mL) and DCM (28 mL). The resulting mixture was cooled to −78° C., O3 was bubbled into the solution for 7 min, N2 was bubbled for 10 min, and then Me2S (14 mL) was added. The reaction mixture was slowly warmed to room temperature and stirred for 20 min. The mixture was concentrated under reduced pressure to provide 2,6-dichloro-N-(2-(cyclopropanecarboxamido)pyridin-4-yl)-4-formylbenzamide (0.70 g, yield: 86%). LCMS (ESI) m/z: 378.1 [M+H+].

후처리

  1. customO3 was bubbled into the solution for 7 min
  2. customN2 was bubbled for 10 min
  3. additionMe2S (14 mL) was added
  4. temperatureThe reaction mixture was slowly warmed to room temperature
  5. concentrationThe mixture was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0aff287a4b6d4fa2a0cca6e23d01d417
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486950B2

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