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

HRID 1648933ノート

反応式

HRID 1648933 の反応式
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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 5083724Palladium monoxide触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4383cb1e7e704faca0488ab4e0b3fa8c
出典データセット
uspto-grants-1983_11
特許番号
US04414225

反応ノート

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