Dichloromethane → HCID 23142599、化合物

HRID 32193ノート

反応式

HRID 32193 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[C:18]([O:20][CH3:21])[C:17]([N:22]3[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]3)=[CH:16][C:15]=2[CH:28]2[CH2:33][C:32]([CH3:35])([CH3:34])[CH2:31][C:30]([CH3:37])([CH3:36])[CH2:29]2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O.ClCCl.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[CH3:21][O:20][C:18]1[C:17]([N:22]2[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27]2)=[CH:16][C:15]([CH:28]2[CH2:29][C:30]([CH3:36])([CH3:37])[CH2:31][C:32]([CH3:35])([CH3:34])[CH2:33]2)=[C:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)[CH:19]=1

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 597693744-[5-Methoxy-4-piperidin-1-yl-2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester

生成物 1

HCID 23142599HCID 23142599、化合物収率 79.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of the 4-[5-methoxy-4-piperidin-1-yl-2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester (88 mg, 0.17 mmol) produced in Example (72a), trifluoroacetic acid (0.25 mL, 3.2 mmol) and dichloromethane (0.5 mL) was stirred for 1 hour and 10 minutes at room temperature. Saturated aqueous solution of sodium hydrogencarbonate was added to the reaction mixture and extraction was performed with ethyl acetate. The separated organic layer was dried over anhydrous sodium sulfate. The desiccant was filtered off and the filtrate was concentrated under reduced pressure. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane) to give 56 mg of the title compound as a red solid.

後処理

  1. dry with materialThe separated organic layer was dried over anhydrous sodium sulfate
  2. filtrationThe desiccant was filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane)

出典と根拠

ORDレコード
ord-c38738af640045bca633ae06ff55ddaf
出典データセット
uspto-grants-2008_09
特許番号
US07425554B2

反応ノート

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