홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Hydrogen Peroxide → HCID 58223423, 화합물

HRID 41256
노트
인쇄 미리보기

반응식

HRID 41256 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 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

생성물 1

HCID 58223423
HCID 58223423, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4ab51766ca7d43a5800ab829a3382bc8
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08530504B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트