Hydrogen Sulfide → HCID 22003635、化合物

HRID 324449

反応式

HRID 324449 の反応式
[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]

参加物

5

反応物 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

生成物 1

HCID 22003635HCID 22003635、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f10df7e12b0b47ecb0ea620d43f44c2e
出典データセット
uspto-grants-2001_04
特許番号
US06218376B1

関連ノート

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