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Triethylamine → N-[3-(3,5-bis(trifluoromethyl)benzyloxy)-2-phenylpropyl]-1-methylpiperidine-4-carboxamide

HRID 548199
ノート
印刷プレビュー

反応式

HRID 548199 の反応式
C[C:2]1([C:8]([OH:10])=O)[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.Cl.[F:12][C:13]([F:37])([F:36])[C:14]1[CH:15]=[C:16]([CH:29]=[C:30]([C:32]([F:35])([F:34])[F:33])[CH:31]=1)[CH2:17][O:18][CH2:19][CH:20]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH2:21][NH2:22].[CH2:38](N(CC)CC)C.CCN=C=NCCCN(C)C.Cl>C(Cl)Cl.O>[F:12][C:13]([F:36])([F:37])[C:14]1[CH:15]=[C:16]([CH:29]=[C:30]([C:32]([F:34])([F:33])[F:35])[CH:31]=1)[CH2:17][O:18][CH2:19][CH:20]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH2:21][NH:22][C:8]([CH:2]1[CH2:3][CH2:4][N:5]([CH3:38])[CH2:6][CH2:7]1)=[O:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 221045794-Methylpiperidine-4-carboxylic acidHCID 866240403-(3,5-Bis(trifluoromethyl)benzyloxy)-2-phenylpropylamine hydrochloride

生成物 1

HCID 86624039N-[3-(3,5-bis(trifluoromethyl)benzyloxy)-2-phenylpropyl]-1-methylpiperidine-4-carboxamide
収率 93%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

4-Methylpiperidine-4-carboxylic acid (0.41 g, 2.9 mmol), the compound produced in Example 17 (0.99 g, 2.9 mmol) and triethylamine (0.40 mL, 2.9 mmol) were dissolved in CH2Cl2 (10 mL) and WSC.HCl (0.56 g, 2.9 mmol) was added thereto at room temperature. After the mixture was stirred for 20 hours at room temperature, water was added to the residue obtained by evaporation of the solvent in vacuo and the mixture was extracted with ethyl acetate. The organic layers were combined, washed with water and a saturated saline solution and dried over anhydrous sodium sulfate. The solvent was evaporated therefrom in vacuo to give Compound 1 (1.12 g, 93%) as an oily product.

後処理

  1. customat room temperature
  2. customobtained by evaporation of the solvent in vacuo
  3. extractionthe mixture was extracted with ethyl acetate
  4. washwashed with water
  5. dry with materiala saturated saline solution and dried over anhydrous sodium sulfate
  6. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-46867278d280445aa02087d1d2a66153
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07939552B2

反応ノート

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