Tetrahydrofuran → 8-Bromo-11-ethyl-5,11-dihydro-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one

HRID 2229303노트

반응식

HRID 2229303 반응식
Cl[C:2]1[C:7]([C:8]([NH:10][C:11]2[C:12]([NH:17][CH2:18][CH3:19])=[N:13][CH:14]=[CH:15][CH:16]=2)=[O:9])=[CH:6][C:5]([Br:20])=[CH:4][N:3]=1.C[Si](C)(C)[N-][Si](C)(C)C.[Na+].C1COCC1>N1C=CC=CC=1>[Br:20][C:5]1[CH:4]=[N:3][C:2]2[N:17]([CH2:18][CH3:19])[C:12]3[N:13]=[CH:14][CH:15]=[CH:16][C:11]=3[NH:10][C:8](=[O:9])[C:7]=2[CH:6]=1

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 2724254Sodium bis(trimethylsilyl)amideHCID 120157285-Bromo-2-chloro-N-[2-(ethylamino)pyridin-3-yl]pyridine-3-carboxamide

생성물 1

HCID 120157298-Bromo-11-ethyl-5,11-dihydro-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one수율 75%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a solution of 2-chloro-N-{2-(ethylamino)-3-pyridinyl}-5-bromo-3-pyridinecarboxamide (54.9 g, 154.4 mmol) in pyridine (308 mL) at 50° C. was added drop-wise a 1 M solution of NaHMDS (sodium hexamethyldisilazide) in THF (355 mL, 355 mmol). After 10 min, the reaction was allowed to cool to room temperature, and then was poured over ice water (2 L). The resulting solid was filtered, rinsed with water and then hexane. The solid was dried under reduced pressure to give the title compound (36 g, 75% yield) as a dark green solid.

후처리

  1. filtrationThe resulting solid was filtered
  2. washrinsed with water
  3. customThe solid was dried under reduced pressure

출처 및 근거

ORD 기록
ord-1d89d4079a874fb8bebf53aab3de110b
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06420359B1

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