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Piperidine, 4-(phenylmethyl)-, hydrochloride (1:1) → HCID 19598360、化合物

HRID 1290064
ノート
印刷プレビュー

反応式

HRID 1290064 の反応式
[C:1]1([N:7]2[CH:11]=[CH:10][C:9]([CH:12]=O)=[CH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:14]([CH:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(C1CCNCC1)C1C=CC=CC=1.Cl.C([BH3-])#N.[Na+]>CO>[C:1]1([N:7]2[CH:11]=[CH:10][C:9]([CH2:12][N:24]3[CH2:25][CH2:26][CH:21]([CH2:14][C:15]4[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=4)[CH2:22][CH2:23]3)=[CH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 31737Piperidine, 4-(phenylmethyl)-, hydrochloride (1:1)HCID 317384-BenzylpiperidineHCID 5003444Sodium cyanoborohydrideHCID 10920962HCID 10920962、化合物

生成物 1

HCID 19598360HCID 19598360、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 171 mg of 1-phenyl pyrrole-3-carboxaldehyde in 1 mL of methanol was added 525 mg of 4-benzylpiperidine, 175 mg of 4-benzylpiperidine·HCl and 63 mg of sodium cyanoborohydride. The reaction mixture was stirred overnight at room temperature under an atmosphere of nitrogen. The methanol was removed by evaporation under reduced pressure and the residue was extracted into 50 mL of ethyl acetate, then washed successively with 50 mL aliquots of 10% sodium hydroxide and water. The ethyl acetate extract was dried over anhydrous sodium sulfate and the solvent evaporated under reduced pressure to yield 1-phenyl-3[(4-benzyl-piperidin-1-yl)methyl]pyrrole, which was purified by chromatography on silica gel using 5% methanol in dichloromethane as elvent. On evaporation of the solvent, the free base was dissolved in ethanol and treated with 1 equivalent of maleic acid. The 1-phenyl-3[(4-benzyl-piperidin-1-yl)methyl]pyrrole maleate salt (compound 7) had a melting point of 159°-161° C.

後処理

  1. customThe methanol was removed by evaporation under reduced pressure
  2. extractionthe residue was extracted into 50 mL of ethyl acetate
  3. washwashed successively with 50 mL aliquots of 10% sodium hydroxide and water
  4. extractionThe ethyl acetate extract
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. customthe solvent evaporated under reduced pressure

出典と根拠

ORDレコード
ord-25163ebdf38545e1accc1e55e08675d2
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05750700

反応ノート

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