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

2-Bromo-4-fluorobenzene-1-sulfonyl chloride → methyl 7-(2-bromo-4-fluorobenzenesulfonylamino)-4H-5-oxa-3,9b-diazacyclopenta[a]naphthalene-6-carboxylate

HRID 595120
ノート
印刷プレビュー

反応式

HRID 595120 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:9]2[N:8]3[CH:12]=[CH:13][N:14]=[C:7]3[CH2:6][O:5][C:4]=2[C:3]=1[C:15]([O:17][CH3:18])=[O:16].[Br:19][C:20]1[CH:25]=[C:24]([F:26])[CH:23]=[CH:22][C:21]=1[S:27](Cl)(=[O:29])=[O:28]>N1C=CC=CC=1.C(Cl)Cl>[Br:19][C:20]1[CH:25]=[C:24]([F:26])[CH:23]=[CH:22][C:21]=1[S:27]([NH:1][C:2]1[CH:11]=[CH:10][C:9]2[N:8]3[CH:12]=[CH:13][N:14]=[C:7]3[CH2:6][O:5][C:4]=2[C:3]=1[C:15]([O:17][CH3:18])=[O:16])(=[O:29])=[O:28]
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 2

HCID 27782162-Bromo-4-fluorobenzene-1-sulfonyl chloride2 回HCID 86712824methyl 7-amino-4H-5-oxa-3,9b-diazacyclopenta[a]naphthalene-6-carboxylate2 回

生成物 1

HCID 70983693methyl 7-(2-bromo-4-fluorobenzenesulfonylamino)-4H-5-oxa-3,9b-diazacyclopenta[a]naphthalene-6-carboxylate収率 80.9%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

A mixture of methyl 7-amino-4H-5-oxa-3,9b-diazacyclopenta[a]naphthalene-6-carboxylate (Intermediate 26, 0.379 g) and 2-bromo-4-fluorobenzenesulfonyl chloride (0.466 g) in pyridine (10 mL) and DCM (10 mL) was stirred at room temperature for 17 hours. A further amount of 2-bromo-4-fluorobenzenesulfonyl chloride (0.190 g) was added and the mixture was stirred at room temperature for 5 hours. The resultant mixture was concentrated in vacuo and the residue was dissolved in DCM and water and passed through a phase separator. The filtrate was concentrated in vacuo and the residue was purified by chromatography on silica, eluting with ethyl acetate to give a white solid which was triturated with ether to give methyl 7-(2-bromo-4-fluorobenzenesulfonylamino)-4H-5-oxa-3,9b-diazacyclopenta[a]naphthalene-6-carboxylate (0.603 g) as an off-white solid.

後処理

  1. stirringthe mixture was stirred at room temperature for 5 hours
  2. concentrationThe resultant mixture was concentrated in vacuo
  3. dissolutionthe residue was dissolved in DCM
  4. concentrationThe filtrate was concentrated in vacuo
  5. customthe residue was purified by chromatography on silica
  6. washeluting with ethyl acetate
  7. customto give a white solid which
  8. customwas triturated with ether

出典と根拠

ORDレコード
ord-debba7d723ce4c44bf68db8943fbc1ea
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09242997B2

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