Hydrochloric Acid → Ethyl 5,6,7,8-tetrahydro-4H-thieno[2,3-d]azepine-2-carboxylate hydrochloride

HRID 1648933노트

반응식

HRID 1648933 반응식
C([N:8]1[CH2:14][CH2:13][C:12]2[CH:15]=[C:16]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[S:17][C:11]=2[CH2:10][CH2:9]1)C1C=CC=CC=1.[ClH:23]>C(O)C.[Pd]=O>[ClH:23].[S:17]1[C:11]2[CH2:10][CH2:9][NH:8][CH2:14][CH2:13][C:12]=2[CH:15]=[C:16]1[C:18]([O:20][CH2:21][CH3:22])=[O:19]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 13072038ethyl 6-benzyl-5,6,7,8-tetrahydro-4H-thieno[2,3-d]azepine-2-carboxylate

생성물 1

HCID 20481328Ethyl 5,6,7,8-tetrahydro-4H-thieno[2,3-d]azepine-2-carboxylate hydrochloride

시약·촉매·용매 2

HCID 5083724Palladium monoxide촉매HCID 702Ethanol용매

실험 절차

15.4 gm (0.049 mol) of ethyl 6-benzyl-5,6,7,8-tetrahydro-4H-thieno[2,3-d]-azepine-2-carboxylate were dissolved in 200 of ethyl alcohol by the addition of 50 ml of 1 N hydrochloric acid. After the addition of 5 gm of palladium oxide, the mixture was hydrogenated in an autoclave for 3 hours at 80° C. and under a hydrogen pressure of 5 bars. After the reaction mixture had been cooled, the catalyst was filtered off, the filtrate was evaporated, and the residue was triturated with acetone. The product was suction-filtered and washed several times with acetone.

후처리

  1. temperatureAfter the reaction mixture had been cooled
  2. filtrationthe catalyst was filtered off
  3. customthe filtrate was evaporated
  4. customthe residue was triturated with acetone
  5. filtrationThe product was suction-filtered
  6. washwashed several times with acetone

출처 및 근거

ORD 기록
ord-4383cb1e7e704faca0488ab4e0b3fa8c
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04414225

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