Hydrochloric Acid → HCID 68496449、化合物

HRID 445245

反応式

HRID 445245 の反応式
C([N:8]1[CH:17]([CH3:18])[CH2:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH:9]1[C:19]1[CH:24]=[CH:23][C:22]([C:25]([F:28])([F:27])[F:26])=[CH:21][CH:20]=1)C1C=CC=CC=1.[ClH:29]>CO.[Pd]>[ClH:29].[CH3:18][CH:17]1[CH2:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH:9]([C:19]2[CH:20]=[CH:21][C:22]([C:25]([F:27])([F:26])[F:28])=[CH:23][CH:24]=2)[NH:8]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 595362822-Benzyl-3-methyl-1-(4-(trifluoromethyl)phenyl)-1,2,3,4-tetrahydroisoquinoline

生成物 1

HCID 68496449HCID 68496449、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒2 回HCID 887Methanol溶媒

実験手順

To a solution of 2-benzyl-3-methyl-1-(4-(trifluoromethyl)phenyl)-1,2,3,4-tetrahydroisoquinoline (485 mg, 1.27 mmol) in MeOH (5 mL) was added palladium, 10 wt. % on activated carbon (41 mg, 0.38 mmol). The resulting mixture was then stirred under H2 for 16 h. Then, 5 N HCl (0.2 mL) was added followed by palladium, 10 wt. % on activated carbon (41 mg, 0.38 mmol). The resulting mixture was stirred at RT under H2 (45 psi) for 30 min. The mixture was filtered through celite and the celite was washed with MeOH (2×5 mL). The combined filtrates were concentrated to give the title compound as a light yellow solid (HCl salt), which was used in the next step without further purification.

後処理

  1. stirringThe resulting mixture was stirred at RT under H2 (45 psi) for 30 min
  2. filtrationThe mixture was filtered through celite
  3. washthe celite was washed with MeOH (2×5 mL)
  4. concentrationThe combined filtrates were concentrated

出典と根拠

ORDレコード
ord-8b290a7c96fc4c3ba073afaa60c6d4c6
出典データセット
uspto-grants-2013_07
特許番号
US08476297B2

関連ノート

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