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

HRID 2229303ノート

反応式

HRID 2229303 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-1d89d4079a874fb8bebf53aab3de110b
出典データセット
uspto-grants-2002_07
特許番号
US06420359B1

反応ノート

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