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Acetyl chloride → HCID 42611207、化合物

HRID 1260933
ノート
印刷プレビュー

反応式

HRID 1260933 の反応式
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([C@H:10]2[C@H:15]([N:16]([CH3:33])[C:17](=[O:32])[C:18]3[CH:23]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:21]=[C:20]([C:28]([F:31])([F:30])[F:29])[CH:19]=3)[CH2:14][CH2:13][N:12]([C:34]([CH:36]3[CH2:41][CH2:40][NH:39][CH2:38][CH2:37]3)=[O:35])[CH2:11]2)[CH:6]=[CH:7][C:8]=1[Cl:9].C(N(CC)CC)C.[C:49](Cl)(=[O:51])[CH3:50].[OH-].[Na+]>C(#N)C.O>[C:49]([N:39]1[CH2:40][CH2:41][CH:36]([C:34]([N:12]2[CH2:13][CH2:14][C@@H:15]([N:16]([CH3:33])[C:17](=[O:32])[C:18]3[CH:23]=[C:22]([C:24]([F:25])([F:27])[F:26])[CH:21]=[C:20]([C:28]([F:29])([F:31])[F:30])[CH:19]=3)[C@H:10]([C:5]3[CH:6]=[CH:7][C:8]([Cl:9])=[C:3]([Cl:2])[CH:4]=3)[CH2:11]2)=[O:35])[CH2:37][CH2:38]1)(=[O:51])[CH3:50]
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 6367Acetyl chlorideHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 86631339N-[(3R,4R)-3-(3,4-dichlorophenyl)-1-(piperidin-4-ylcarbonyl)piperidin-4-yl]-N-methyl-3,5-bis(trifluoromethyl)benzamide Monohydrochloride

生成物 1

HCID 42611207HCID 42611207、化合物収率 71%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6342Acetonitrile溶媒

実験手順

To a solution of N-[(3R,4R)-3-(3,4-dichlorophenyl)-1-(piperidin-4-ylcarbonyl)piperidin-4-yl]-N-methyl-3,5-bis(trifluoromethyl)benzamide monohydrochloride (0.35 g) obtained in Example 89 and triethylamine (0.24 mL) in acetonitrile (10 mL) was added acetyl chloride (0.080 mL) at 0° C., and the mixture was stirred at room temperature for 14 hr. The reaction mixture was poured into water, the mixture was made basic with 2N aqueous sodium hydroxide solution, and the resultant product was extracted with ethyl acetate. The organic layer was washed with aqueous sodium hydrogen carbonate solution and brine and dried, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH Chromatorex) (solvent gradient; 75→100% ethyl acetate/hexane) to give the title compound (0.25 g, 71%) as a white crystal powder.

後処理

  1. extractionthe resultant product was extracted with ethyl acetate
  2. washThe organic layer was washed with aqueous sodium hydrogen carbonate solution and brine
  3. customdried
  4. customthe solvent was evaporated under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography (NH Chromatorex) (solvent gradient; 75→100% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-412b4328d9ca458e98fabdb7eaa19278
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08470816B2

反応ノート

読み込み中…

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