Potassium ethanethioate → HCID 86749918、化合物

HRID 864511ノート

反応式

HRID 864511 の反応式
[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]

参加物

4

反応物 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

生成物 1

HCID 86749918HCID 86749918、化合物収率 97.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fd8b095a20c04b00982a1f3983b569cf
出典データセット
uspto-grants-1996_10
特許番号
US05563137

反応ノート

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