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

Hydrochloric Acid → Benzenesulfonamide

HRID 1262814
ノート
印刷プレビュー

反応式

HRID 1262814 の反応式
C[NH:2][S:3]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1C)(=[O:5])=[O:4].C([Li])CCC.C[Sn](Cl)(C)C.Cl>O1CCCC1>[C:6]1([S:3]([NH2:2])(=[O:5])=[O:4])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=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 313Hydrochloric AcidHCID 14016Trimethyltin chlorideHCID 10197977N-Methyl-o-toluenesulfonamideHCID 178418339Butyllithium

生成物 1

HCID 7370Benzenesulfonamide収率 108.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of N,2-dimethylbenzenesulfonamide (3.70 g, 20.0 mmol) in dry tetrahydrofuran (75 ml) was cooled to -78° with stirring under nitrogen. n-Butyllithium in hexanes (1.6 M, 28 ml, 44 mmol) was added dropwise over 1/2 hour. After 2 hours at -78°, a solution of trimethyltin chloride (4.42 g, 22.0 mmol) in dry tetrahydrofuran (20 ml) was added dropwise. The reaction mixture was allowed to warm to 0° over 1 hour, and then 5% HCl (50 ml) was added dropwise at a rate to maintain an internal temperature less than 10°. After concentrating the reaction mixture in vacuo, the product was extracted into methylene chloride (3×100 ml), washed with water (2×200 ml), dried (MgSO4), filtered and concentrated. Purification by flash chromatography (SiO2, hexane/ethyl acetate, 8:2) gave N-methyl-2-[(trimethylstannyl)methyl)]benzenesulfonamide (3.4 g, 49%) as a white powder, m.p. 59° -60°.

後処理

  1. temperatureto warm to 0° over 1 hour
  2. temperatureto maintain an internal temperature less than 10°
  3. concentrationAfter concentrating the reaction mixture in vacuo
  4. extractionthe product was extracted into methylene chloride (3×100 ml)
  5. washwashed with water (2×200 ml)
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customPurification by flash chromatography (SiO2, hexane/ethyl acetate, 8:2)

出典と根拠

ORDレコード
ord-27bbcadbab9743c6b00eb081aa5ca720
出典データセット
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04454135

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