Hydrochloric Acid → HCID 15524296、化合物

HRID 322229ノート

反応式

HRID 322229 の反応式
Cl.C([NH:5][C:6]1[C:11]2[C:12](=[O:20])[C:13]3[S:19][CH:18]=[CH:17][C:14]=3[CH2:15][S:16][C:10]=2[CH:9]=[CH:8][CH:7]=1)(=O)C.C(=O)([O-])O.[Na+]>CO>[NH2:5][C:6]1[C:11]2[C:12](=[O:20])[C:13]3[S:19][CH:18]=[CH:17][C:14]=3[CH2:15][S:16][C:10]=2[CH:9]=[CH:8][CH:7]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 155242959-Acetamido-4,10-dihydrothieno[3,2-c][1]benzothiepin-10-one

生成物 1

HCID 15524296HCID 15524296、化合物収率 99%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In a mixed solvent of methanol (15 ml) and concentrated hydrochloric acid (15 ml), 9-acetamido-4,10-dihydrothieno[3,2-c][1]benzothiepin-10-one obtained in Reference Example 4 (0.74 g, 2.5 mmol) was heated under reflux for one hour. The reaction mixture was poured into a saturated aqueous solution of sodium hydrogen carbonate, followed by extraction with ethyl acetate (25 ml). The organic layer was washed with a saturated aqueous solution of sodium chloride, and then dried over anhydrous magnesium sulfate. After the drying agent was filtered off, the organic layer was concentrated under reduced pressure to give 9-amino-4,10-dihydrothieno[3,2-c][1]benzothiepin-10-one as a yellow solid (0.6 g, 99%).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for one hour
  3. extractionfollowed by extraction with ethyl acetate (25 ml)
  4. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationAfter the drying agent was filtered off
  7. concentrationthe organic layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-12e7e31d92164f6582278df398a5a13e
出典データセット
uspto-grants-2001_04
特許番号
US06211227B1

反応ノート

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