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 Hydroxide → HCID 136348379、化合物

HRID 1777072
ノート
印刷プレビュー

反応式

HRID 1777072 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([OH:13])=[C:6](/[CH:8]=[C:9](\[CH3:12])/[CH:10]=O)[CH:7]=1.CC1C=CC(S([NH:24][NH2:25])(=O)=O)=CC=1.[OH-].[Na+].[O:28]1[CH2:33][CH2:32][N:31]([S:34]([C:37]2[CH:38]=[C:39]([CH:43]=[CH:44][CH:45]=2)[C:40](Cl)=[O:41])(=[O:36])=[O:35])[CH2:30][CH2:29]1>C(#N)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([OH:13])=[C:6]([C:8]2[C:9]([CH3:12])=[CH:10][N:25]([C:40]([C:39]3[CH:43]=[CH:44][CH:45]=[C:37]([S:34]([N:31]4[CH2:32][CH2:33][O:28][CH2:29][CH2:30]4)(=[O:36])=[O:35])[CH:38]=3)=[O:41])[N:24]=2)[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 14798Sodium Hydroxide2 回HCID 15303P-ToluenesulfonylhydrazideHCID 5426758(2E)-3-(5-Chloro-2-hydroxyphenyl)-2-methylacrylaldehydeHCID 18801891HCID 18801891、化合物

生成物 1

HCID 136348379HCID 136348379、化合物収率 31.5%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒
2 回

実験手順

A mixture of (E)-3-(5-chloro-2-hydroxyphenyl)-2-methylacrylaldehyde (40 mg, 0.203 mmol) and 4-methylbenzenesulfonohydrazide (41.7 mg, 0.224 mmol) in Acetonitrile (3 mL) were stirred at room temperature for 3 h and then acetonitrile (2 mL), Sodiumhydroxide (8.95 mg, 0.224 mmol) were added and the mixture was heated at reflux for 16 h, then Sodiumhydroxide (12.21 mg, 0.305 mmol) and 3-(morpholinosulfonyl)benzoyl chloride (88 mg, 0.305 mmol) (made from 3-(morpholinosufonyl)benzoic acid) were subsequently added and the mixture was stirred at room temperature for 2 h. Reaction was monitored by TLC. After completion of the reaction, the product was extracted with EtOAc and the organic layer was washed with brine, dried over anhydrous Na2SO4, filtered, and solvent was removed by vacuum. The resulting crude material was purified by flash column chromatography (2% CH3OH/CH2Cl2) afforded the desired product (3-(5-chloro-2-hydroxyphenyl)-4-methyl-1H-pyrazol-1-yl)(3-(morpholinosulfonyl)phenyl)methanone (30 mg, 0.064 mmol, 31.3% yield) as a solid. 1HNMR (400 MHz, CDCl3): δ 8.28 (m, 2H), 8.20 (d, 1H, J=8.0 Hz), 7.95 (d, 1H, J=8.4 Hz), 7.70 (t, 1H, J=7.6 Hz), 7.59 (d, 1H, J=2.4 Hz), 7.18 (dd, 1H, J=2.8 & 8.8 Hz), 6.87 (d, 1H, J=8.4 Hz), 3.68 (m, 4H), 3.02 (m, 4H), 2.40 (s, 3H). ESI-MS: 462.0 [M+H]+

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 16 h
  3. stirringthe mixture was stirred at room temperature for 2 h
  4. customReaction
  5. customAfter completion of the reaction
  6. extractionthe product was extracted with EtOAc
  7. washthe organic layer was washed with brine
  8. dry with materialdried over anhydrous Na2SO4
  9. filtrationfiltered
  10. customsolvent was removed by vacuum
  11. customThe resulting crude material was purified by flash column chromatography (2% CH3OH/CH2Cl2)

出典と根拠

ORDレコード
ord-4edcf96539fa4ca3bc0960f69f92b27f
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09266838B2

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