Potassium ethanethioate → HCID 86749918, 화합물

HRID 864511노트

반응식

HRID 864511 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:10][C@H:9]3[C@@H:11]([O:30][C:31](=[O:33])[CH3:32])[C@@H:12]([O:26][C:27](=[O:29])[CH3:28])[C@@H:13](OS(C4C=CC(C)=CC=4)(=O)=O)[O:14][C@H:8]3[N:7]([CH2:34][CH2:35][N:36]([CH2:39][CH3:40])[CH2:37][CH3:38])[C:6]=2[CH:41]=1.[C:42]([O-:45])(=[S:44])[CH3:43].[K+]>CC(C)=O>[C:42]([S:44][C@H:13]1[O:14][C@@H:8]2[C@@H:9]([S:10][C:5]3[CH:4]=[CH:3][C:2]([Cl:1])=[CH:41][C:6]=3[N:7]2[CH2:34][CH2:35][N:36]([CH2:37][CH3:38])[CH2:39][CH3:40])[C@@H:11]([O:30][C:31](=[O:33])[CH3:32])[C@H:12]1[O:26][C:27](=[O:29])[CH3:28])(=[O:45])[CH3:43]

참가 물질

4

반응물 2

HCID 23670855Potassium ethanethioateHCID 86749916(2R, 3R, 4S, 4aS, 10aR)-8-chloro-3, 4-diacetoxy-10-(2-diethylaminoethyl)-2-(4-methylphenylsulfonyloxy)-2, 3, 4, 4a, 10, 10a-hexahydropyrano [3, 2-b] [1, 4] benzothiazine

생성물 1

HCID 86749918HCID 86749918, 화합물수율 97.4%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To the solution of 2.0 g of the compound (36) obtained in Example 35 in 100 ml of acetone, 1.0 g of potassium thioacetate was added, and the mixture was heated with refluxing for 6.5 hours. The solvent was removed under reduced pressure, and the residue was dissolved in ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to obtain 1.65 g (yield 96.8% ) of the title compound.

후처리

  1. temperaturethe mixture was heated
  2. temperaturewith refluxing for 6.5 hours
  3. customThe solvent was removed under reduced pressure
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. washThe organic layer was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-fd8b095a20c04b00982a1f3983b569cf
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05563137

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