Hydrochloric Acid → HCID 15524296, 화합물

HRID 322229노트

반응식

HRID 322229 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 15524296HCID 15524296, 화합물수율 99%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-12e7e31d92164f6582278df398a5a13e
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211227B1

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