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 → (5-Bromo-1-isopropyl-1H-pyrazol-4-YL)methanol

HRID 537094
ノート
印刷プレビュー

反応式

HRID 537094 の反応式
[Br:1][C:2]1[N:6]([CH:7]([CH3:9])[CH3:8])[N:5]=[CH:4][C:3]=1[C:10](OCC)=[O:11].B.CSC.[OH-].[Na+]>CC1CCCO1>[Br:1][C:2]1[N:6]([CH:7]([CH3:8])[CH3:9])[N:5]=[CH:4][C:3]=1[CH2:10][OH:11]
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 14798Sodium HydroxideHCID 12423031(Dimethyl sulfide)trihydroboron2 回HCID 67491431Ethyl 5-bromo-1-isopropyl-1H-pyrazole-4-carboxylate

生成物 1

HCID 67491477(5-Bromo-1-isopropyl-1H-pyrazol-4-YL)methanol収率 65%

試薬・触媒・溶媒 1

HCID 73012-Methyltetrahydrofuran溶媒

実験手順

To a solution of ethyl 5-bromo-1-isopropyl-1H-pyrazole-4-carboxylate (163 g, 0.50 mol) in 2-methyl tetrahydrofuran (400 mL) was added borane-DMS (140 mL, 1.50 mol) at 0° C., under argon (effervescence ceased after 50 mL was added). The mixture was stirred at room temperature for 30 minutes and then heated to 70° C. for 2 hours, and then to reflux for 17 hours. Additional portion of borane DMS (40 mL) was added and the mixture was stirred at reflux for an additional 3 hours. The mixture was cooled to room temperature then added gradually to ice-cold methanol (500 mL) with stirring, over a period of 30 minutes. The mixture was stirred at room temperature for 30 minutes then 2 M aqueous sodium hydroxide (1.5 L) was added. The layers were separated and the aqueous layer was extracted with ethyl acetate (2×500 mL). The organic layers were combined, washed with brine (500 mL), dried over magnesium sulfate, filtered and the solvent removed in vacuo. The crude product was purified by dry flash chromatography (0-50% ethyl acetate in heptane) to give (5-bromo-1-isopropyl-1H-pyrazol-4-yl)methanol (70.8 g, 65% over two steps). +ESI (M+H) 220.9; 1H NMR (400 MHz, CDCl3, δ): 7.52 (s, 1H), 4.67 (m, 1H), 4.47 (s, 2H), 2.59 (br. s., 1H), 1.41 (s, 6H).

後処理

  1. temperatureheated to 70° C. for 2 hours
  2. temperatureto reflux for 17 hours
  3. stirringthe mixture was stirred
  4. temperatureat reflux for an additional 3 hours
  5. temperatureThe mixture was cooled to room temperature
  6. stirringwith stirring, over a period of 30 minutes
  7. stirringThe mixture was stirred at room temperature for 30 minutes
  8. customThe layers were separated
  9. extractionthe aqueous layer was extracted with ethyl acetate (2×500 mL)
  10. washwashed with brine (500 mL)
  11. dry with materialdried over magnesium sulfate
  12. filtrationfiltered
  13. customthe solvent removed in vacuo
  14. customThe crude product was purified
  15. dry with materialby dry flash chromatography (0-50% ethyl acetate in heptane)

出典と根拠

ORDレコード
ord-fb143f7b265c4e67a741db70257adfee
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08859773B2

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