Hydrogen Sulfide → HCID 22003635, 화합물

HRID 324449

반응식

HRID 324449 반응식
[SH2:1].CC(C)([O-])C.[K+].[CH2:8]([C:10]1O[C:12]2[CH2:19][CH2:18][C:17]3[CH:20]=[C:21]([CH3:24])[CH:22]=[CH:23][C:16]=3[C:15](=[O:25])[C:13]=2[N:14]=1)[CH3:9]>CN(C)C=O>[CH2:8]([C:10]1[S:1][C:12]2[CH2:19][CH2:18][C:17]3[CH:20]=[C:21]([CH3:24])[CH:22]=[CH:23][C:16]=3[C:15](=[O:25])[C:13]=2[N:14]=1)[CH3:9]

참가 물질

5

반응물 3

HCID 402Hydrogen SulfideHCID 220036422-Ethyl-9,10-dihydro-7-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-oneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 22003635HCID 22003635, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Hydrogen sulphide was passed through a suspension of potassium tert-butoxide (9.31 g) in N,N-dimethylformamide (80 ml) at 5° C. until the mixture was saturated. The product from example 1 step (v) (5.0 g) was added and the reaction mixture stirred at room temperature for 2 h. The mixture was poured onto ice, acidified to pH3 and extracted with ethyl acetate. The organic phase was washed with water, dried (MgSO4) and evaporated under reduced pressure. Purification was by chromatography eluting with 40-50% ethyl acetate in isohexane.

후처리

  1. additionThe mixture was poured onto ice
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed with water
  4. dry with materialdried (MgSO4)
  5. customevaporated under reduced pressure
  6. customPurification
  7. washeluting with 40-50% ethyl acetate in isohexane

출처 및 근거

ORD 기록
ord-f10df7e12b0b47ecb0ea620d43f44c2e
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06218376B1

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