Water → HCID 22563219、化合物

HRID 982714ノート

反応式

HRID 982714 の反応式
[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

参加物

7

反応物 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

生成物 1

HCID 22563219HCID 22563219、化合物収率 94.9%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-ac5a25c1784e408195cc460a0be4a7b0
出典データセット
uspto-grants-2005_03
特許番号
US06861438B2

反応ノート

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