Hydrochloric Acid → 7-(4-ethoxyphenyl)-N-[4-[N-methyl-N-(4-oxocyclohexyl)aminomethyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide

HRID 1978557노트

반응식

HRID 1978557 반응식
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[CH:12][C:13]3[S:19](=[O:21])(=[O:20])[CH2:18][CH2:17][C:16]([C:22]([NH:24][C:25]4[CH:30]=[CH:29][C:28]([CH2:31][N:32]([CH:34]5[CH2:39][CH2:38][C:37]6(OCC[O:40]6)[CH2:36][CH2:35]5)[CH3:33])=[CH:27][CH:26]=4)=[O:23])=[CH:15][C:14]=3[CH:44]=2)=[CH:6][CH:5]=1)[CH3:2].Cl.C(=O)(O)[O-].[Na+]>C1COCC1>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[CH:12][C:13]3[S:19](=[O:21])(=[O:20])[CH2:18][CH2:17][C:16]([C:22]([NH:24][C:25]4[CH:26]=[CH:27][C:28]([CH2:31][N:32]([CH3:33])[CH:34]5[CH2:39][CH2:38][C:37](=[O:40])[CH2:36][CH2:35]5)=[CH:29][CH:30]=4)=[O:23])=[CH:15][C:14]=3[CH:44]=2)=[CH:6][CH:5]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 21995979HCID 21995979, 화합물

생성물 1

HCID 219959207-(4-ethoxyphenyl)-N-[4-[N-methyl-N-(4-oxocyclohexyl)aminomethyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide수율 77.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 7-(4-ethoxyphenyl)-N-[4-[N-(4,4-ethylenedioxycyclohexyl)-N-methylaminomethyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (140 mg) in THF (20 ml) was added at room temperature 3N hydrochloric acid (1 ml), and the mixture was stirred for 40 hours. To the mixture was added saturated sodium bicarbonate solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried with magnesium sulfate and concentrated under reduced pressure to give colorless solid, which was recrystallized from ethyl acetate/hexane to give colorless crystals of 7-(4-ethoxyphenyl)-N-[4-[N-methyl-N-(4-oxocyclohexyl)aminomethyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (Compound 19) (101.1 mg).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried with magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto give colorless solid, which
  6. customwas recrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-95fe5b75bec341a193b03d81d3f9faba
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235771B1

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