ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Formaldehyde → 5-[(2,5-difluorophenyl)[(4-fluorophenyl)sulfonyl]methyl]-N-(dimethylaminomethyl)-4-methylpyridine-2-carboxamide

HRID 1641748
ノート
印刷プレビュー

反応式

HRID 1641748 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH:9]([S:20]([C:23]1[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=1)(=[O:22])=[O:21])[C:10]1[C:11]([CH3:19])=[CH:12][C:13]([C:16]([NH2:18])=[O:17])=[N:14][CH:15]=1.[CH2:30]=O.Cl.[CH3:33][NH:34][CH3:35].O>CN(C)C=O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH:9]([S:20]([C:23]1[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=1)(=[O:22])=[O:21])[C:10]1[C:11]([CH3:19])=[CH:12][C:13]([C:16]([NH:18][CH2:33][N:34]([CH3:30])[CH3:35])=[O:17])=[N:14][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 712FormaldehydeHCID 962WaterHCID 10473Dimethylamine, hydrochlorideHCID 577364915-[(2,5-Difluorophenyl)[(4-fluorophenyl)sulfonyl]methyl]-4-methylpyridine-2-carboxamide

生成物 1

HCID 577364565-[(2,5-difluorophenyl)[(4-fluorophenyl)sulfonyl]methyl]-N-(dimethylaminomethyl)-4-methylpyridine-2-carboxamide収率 63%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 5-[(2,5-difluorophenyl)[(4-fluorophenyl)sulfonyl]methyl]-4-methylpyridine-2-carboxamide (150 mg, 0.33 mmol) obtained in Example 15 in N,N-dimethylformamide (3 ml), a formaldehyde solution (37%, 54 μl) and dimethylamine hydrochloride (136 mg, 1.67 mmol) were added at 0° C., and the mixture was stirred for 2 hours at room temperature. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate, and was dried over anhydrous sodium sulfate. The solvent was concentrated under reduced pressure, and the resulting residue was subjected to silica gel chromatography. The fraction obtained from an elution with dichloromethane:methanol=10:1 was concentrated under reduced pressure, and the resulting residue was washed with diethyl ether and dichloromethane and dried, to obtain the title compound (99 mg, 0.21 mmol, 63%) as a white solid.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialwas dried over anhydrous sodium sulfate
  3. concentrationThe solvent was concentrated under reduced pressure
  4. customThe fraction obtained from an elution with dichloromethane
  5. concentrationmethanol=10:1 was concentrated under reduced pressure
  6. washthe resulting residue was washed with diethyl ether and dichloromethane
  7. customdried

出典と根拠

ORDレコード
ord-a55462c74674461b9dccc5f1b92f632c
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08114886B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート