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

Pyridine → 2-{4-[5-(4-Chlorophenyl)pyrazin-2-ylethynyl]phenoxy}ethyl methanesulfonate

HRID 734882
ノート
印刷プレビュー

反応式

HRID 734882 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[N:14]=[CH:15][C:16]([C:19]#[C:20][C:21]3[CH:30]=[CH:29][C:24]([O:25][CH2:26][CH2:27][OH:28])=[CH:23][CH:22]=3)=[N:17][CH:18]=2)=[CH:9][CH:8]=1.N1C=CC=CC=1>C(Cl)Cl>[CH3:1][S:2]([O:28][CH2:27][CH2:26][O:25][C:24]1[CH:23]=[CH:22][C:21]([C:20]#[C:19][C:16]2[CH:15]=[N:14][C:13]([C:10]3[CH:9]=[CH:8][C:7]([Cl:6])=[CH:12][CH:11]=3)=[CH:18][N:17]=2)=[CH:30][CH:29]=1)(=[O:4])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049Pyridine2 回HCID 31297Methanesulfonyl chloride2 回HCID 690588142-{4-[5-(4-Chlorophenyl)pyrazin-2-ylethynyl]phenoxy}ethanol

生成物 1

HCID 866011392-{4-[5-(4-Chlorophenyl)pyrazin-2-ylethynyl]phenoxy}ethyl methanesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

0.62 mL (7.98 mmol) of methanesulfonic acid chloride was added dropwise at RT to a solution of 700 mg (2.00 mmol) of 2-{4-[5-(4-chlorophenyl)pyrazin-2-ylethynyl]phenoxy}ethanol and 0.65 mL (7.98 mmol) of pyridine in 20 mL of DCM and the mixture was then stirred overnight at RT. After the addition of another 0.33 mL (3.99 mmol) of pyridine and 0.32 mL (4.12 mmol) of methanesulfonic acid chloride, the reaction mixture was stirred for a further 2 hours at RT in the ultrasound bath. The solution was diluted with 30 mL DCM, and the organic phase was separated off, washed three times with 60 mL of water, and dried over magnesium sulfate. After the desiccant and solvent had been eliminated, the residue was purified by chromatography (silica gel, DCM). Yield: 600 mg (70% of theoretical); C21H17ClN2O4S (M=428.889); calc.: molpeak (M+H)+:429/431 (Cl); found: molpeak (M+H)+:429/431 (Cl); Rf value: 0.30 (silica gel, DCM/MeOH 9:1).

後処理

  1. stirringthe reaction mixture was stirred for a further 2 hours at RT in the ultrasound bath
  2. customthe organic phase was separated off
  3. washwashed three times with 60 mL of water
  4. dry with materialdried over magnesium sulfate
  5. customthe residue was purified by chromatography (silica gel, DCM)

出典と根拠

ORDレコード
ord-50fd1c17ed094f2bb6cdc21cfdd0379b
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07592358B2

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