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

Hydrogen Peroxide → HCID 58223423、化合物

HRID 41256
ノート
印刷プレビュー

反応式

HRID 41256 の反応式
C([C:3]1[C:4]([CH3:18])=[N:5][N:6]2[C:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[C:9]([S:16][CH3:17])[S:8][C:7]=12)=O.[Mn]([O-])(=O)(=O)=O.[K+].[OH:25]O.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=O)C=CC=CC=1.C([N:46]([CH2:49]C)CC)C.[C:51]([OH:55])([CH3:54])([CH3:53])[CH3:52]>C1(C)C=CC=CC=1.CC(C)=O>[C:51]([O:55][C:49]([NH:46][C:3]1[C:4]([CH3:18])=[N:5][N:6]2[C:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[C:9]([S:16][CH3:17])[S:8][C:7]=12)=[O:25])([CH3:54])([CH3:53])[CH3:52]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 784Hydrogen PeroxideHCID 6386tert-ButanolHCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 516875Potassium PermanganateHCID 3507588Ethyl 7-formyl-6-methyl-2-(methylsulfanyl)pyrazolo[5,1-b][1,3]thiazole-3-carboxylate

生成物 1

HCID 58223423
HCID 58223423、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 1140Toluene溶媒

実験手順

To an acetone (7 mL) solution of ethyl 7-formyl-6-methyl-2-(methylthio)pyrazolo[5,1-b][1,3]thiazole-3-carboxylate (100 mg, 0.35 mmol), was added aqueous (3 mL) solution of potassium permanganate (83.4 mg, 0.53 mmol), and the mixture was stirred at room temperature for 45 minutes. To the reaction mixture, aqueous hydrogen peroxide was added, and insoluble matters were filtered off and then the organic solvent in the filtrate was distilled off under reduced pressure. The residue was subjected to cotton filtration, and a 2N aqueous solution of hydrochloric acid was added thereto to yield a solid, the obtained solid was filtered and dried. To a toluene (2 mL) solution of the obtained white solid (80.3 mg, 0.27 mmol) were added diphenylphosphoryl azide (63.1 μL, 0.29 mmol), triethylamine (44.7 μL, 0.32 mmol) and tert-butyl alcohol (122 μL, 1.33 mmol), and the mixture was stirred at 110° C. for two hours. The solvent in the reaction mixture was distilled off under reduced pressure, and the residue was purified by medium pressure silica gel column chromatography (n-heptane/ethyl acetate: 25% then 66%) to obtain 35.7 mg (0.096 mmol) of the title compound.

後処理

  1. filtrationinsoluble matters were filtered off
  2. distillationthe organic solvent in the filtrate was distilled off under reduced pressure
  3. filtrationThe residue was subjected to cotton filtration
  4. additiona 2N aqueous solution of hydrochloric acid was added
  5. customto yield a solid
  6. filtrationthe obtained solid was filtered
  7. customdried
  8. stirringthe mixture was stirred at 110° C. for two hours
  9. distillationThe solvent in the reaction mixture was distilled off under reduced pressure
  10. customthe residue was purified by medium pressure silica gel column chromatography (n-heptane/ethyl acetate

出典と根拠

ORDレコード
ord-4ab51766ca7d43a5800ab829a3382bc8
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08530504B2

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