Water → HCID 22563219, 화합물

HRID 982714노트

반응식

HRID 982714 반응식
[Cl:1][C:2]1[CH:30]=[CH:29][C:5]([CH2:6][NH:7][C:8]([C:10]2[C:11](=[O:28])[C:12]3[S:25][C:24]([CH2:26]O)=[CH:23][C:13]=3[N:14]([CH2:16][C:17]([N:19]([O:21][CH3:22])[CH3:20])=[O:18])[CH:15]=2)=[O:9])=[CH:4][CH:3]=1.N1C(C)=CC(C)=CC=1C.CS([Cl:44])(=O)=O.O>CN(C1C=CN=CC=1)C.CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][NH:7][C:8]([C:10]2[C:11](=[O:28])[C:12]3[S:25][C:24]([CH2:26][Cl:44])=[CH:23][C:13]=3[N:14]([CH2:16][C:17]([N:19]([O:21][CH3:22])[CH3:20])=[O:18])[CH:15]=2)=[O:9])=[CH:29][CH:30]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 79532,4,6-TrimethylpyridineHCID 31297Methanesulfonyl chlorideHCID 22563215N-(4-chlorobenzyl)-2-(hydroxymethyl)-4-{2-[methoxy(methyl)amino]-2-oxoethyl}-7-oxo-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide

생성물 1

HCID 22563219HCID 22563219, 화합물수율 94.9%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6228Dimethylformamide용매

실험 절차

To a mixture of N-(4-chlorobenzyl)-2-(hydroxymethyl)-4-{2-[methoxy(methyl)amino]-2-oxoethyl}-7-oxo-4,7-dihydrothieno [3,2-b]pyridine-6-carboxamide (80 mg, 0.18 mmol), collidine (59 μL, 0.44 mmol) and DMAP (3.2 mg) in DMF (2.6 mL) was added methanesulfonyl chloride (35 μL, 0.44 mmol). The reaction was stirred at room temperature for 24 hrs, then cooled to 0° C. before the addition of water (5 mL). The resulting ppt was collected by filtration and washed with water and dried in vacuo, leaving the title compound as an off-white solid (80 mg). The title compound is also a compound of formula I.

후처리

  1. filtrationThe resulting ppt was collected by filtration
  2. washwashed with water
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-ac5a25c1784e408195cc460a0be4a7b0
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06861438B2

반응 노트

불러오는 중…