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

Sodium hydride → N-(2,6-dichloro-5-fluoro-pyrimidin-4-yl)-N-methyl-methanesulfonamide

HRID 415432
ノート
印刷プレビュー

反応式

HRID 415432 の反応式
[H-].[Na+].[CH3:3][NH:4][S:5]([CH3:8])(=[O:7])=[O:6].[Cl:9][C:10]1[N:15]=[C:14]([Cl:16])[C:13]([F:17])=[C:12](Cl)[N:11]=1>CN(C=O)C.C1COCC1>[Cl:9][C:10]1[N:11]=[C:12]([N:4]([CH3:3])[S:5]([CH3:8])(=[O:7])=[O:6])[C:13]([F:17])=[C:14]([Cl:16])[N: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 3

HCID 24758Sodium hydrideHCID 97632N-MethylmethanesulfonamideHCID 133889932,4,6-Trichloro-5-fluoropyrimidine

生成物 1

HCID 86624844N-(2,6-dichloro-5-fluoro-pyrimidin-4-yl)-N-methyl-methanesulfonamide収率 64%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回
HCID 8028
Tetrahydrofuran
溶媒

実験手順

To a solution of NaH (60% in mineral oil, 176 mg, 8.58 mmol) in anhydrous DMF (2 mL), N-methylmethanesulfonamide (436 mg, 4.0 mmol) in DMF (2 ml) was added. This reaction mixture was stirred for 30 min at room temperature and then added dropwise to the solution of 2,4,6-trichloro-5-fluoropyrimidine (804 mg, 4.0 mmol) in THF (30 ml) at 0° C. The reaction mixture was stirred from 0° C. to room temperature overnight. The solvent was evaporated and the residue was purified by silica gel chromatography (by ISCO Combiflash with gradient 0-30% ethyl acetate in Hexane with 1% TEA. A white solid (700 mg) was obtained, yield 64%. NMR (400 MHz, DMSO) 83.38 (s, 3H), 3.31 (s, 3H).

後処理

  1. stirringThe reaction mixture was stirred from 0° C. to room temperature overnight
  2. customThe solvent was evaporated
  3. customthe residue was purified by silica gel chromatography (by ISCO Combiflash with gradient 0-30% ethyl acetate in Hexane with 1% TEA

出典と根拠

ORDレコード
ord-9715fa285112424ea9b64663547d55bc
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08088784B2

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