Piperidine → Phenylmethyl alpha-[[[2-(diethylamino)ethyl]thio]methyl]benzenepropanoate

HRID 375842

反応式

HRID 375842 の反応式
[CH2:1]=[C:2]([CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:3]([O:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:4].Cl.[CH2:21]([N:23]([CH2:27][CH3:28])[CH2:24][CH2:25][SH:26])[CH3:22].N1CCCCC1.[OH-].C([N+](C)(C)C)C1C=CC=CC=1>CO>[CH2:21]([N:23]([CH2:27][CH3:28])[CH2:24][CH2:25][S:26][CH2:1][CH:2]([CH2:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[C:3]([O:5][CH2:6][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1)=[O:4])[CH3:22]

参加物

6

反応物 4

HCID 8082PiperidineHCID 16031Ethanethiol, 2-(diethylamino)-, hydrochloride (1:1)HCID 66854Benzyltrimethylammonium hydroxideHCID 10912012Benzyl 2-Benzylacrylate

生成物 1

HCID 19937709Phenylmethyl alpha-[[[2-(diethylamino)ethyl]thio]methyl]benzenepropanoate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The oil prepared in Step 10 (1.5 g, 5.95 mmol) is dissolved under argon in methanol (22 mL). To this solution is added 2-diethylaminoethanethiol hydrochloride (1 g, 5.95 mmol), piperidine (0.78 mL, 7.85 mmol) and benzyltrimethylammonium hydroxide (0.25 mL, 0.6 mmol) , and the mixture is stirred at room temperature for 16 hours. The solvent is removed on a rotary evaporator and then the residue is purified by flash chromotography on silica gel to give the pure title compound.

後処理

  1. customThe solvent is removed on a rotary evaporator
  2. customthe residue is purified by flash chromotography on silica gel

出典と根拠

ORDレコード
ord-334a18af66234b7a8a23fa306b8c14f5
出典データセット
uspto-grants-1996_01
特許番号
US05488066

関連ノート

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