Hydrochloric Acid → 7-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol4-one

HRID 324417

반응식

HRID 324417 반응식
CC(C)([O-])C.[K+].[SH2:7].[CH2:8]([C:10]1[CH:11]=[CH:12][C:13]2[C:23](=[O:24])[C:18]3[N:19]=[C:20]([CH3:22])O[C:17]=3[CH2:16][CH2:15][C:14]=2[CH:25]=1)[CH3:9].Cl>CN(C)C=O>[CH2:8]([C:10]1[CH:11]=[CH:12][C:13]2[C:23](=[O:24])[C:18]3[N:19]=[C:20]([CH3:22])[S:7][C:17]=3[CH2:16][CH2:15][C:14]=2[CH:25]=1)[CH3:9]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 402Hydrogen SulfideHCID 220035847-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-oneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 220036117-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol4-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A stirred suspension of potassium tert-butoxide (1.80 g) in dry N,N-dimethylformamide (20 ml) was cooled to 5° C. and saturated with hydrogen sulphide. The product from example 3 step (vi) (1.00 g) was added and the reaction stirred at room temperature for 1 hour. The mixture was poured into ice, acidified to pH4 with 2N hydrochloric acid and extracted with ethyl acetate. The extracts were washed with brine, dried (MgSO4) and evaporated to give an orange solid which was purified by chromatography eluting with 50% ethyl acetate in isohexane.

후처리

  1. additionThe mixture was poured into ice
  2. extractionextracted with ethyl acetate
  3. washThe extracts were washed with brine
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customto give an orange solid which
  7. customwas purified by chromatography
  8. washeluting with 50% ethyl acetate in isohexane

출처 및 근거

ORD 기록
ord-adbaab83bb094bc6ab27259c64182025
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06218376B1

연결된 노트

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