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Water → 4-(4-Nitro-3-trifluoromethyl-phenylamino)-piperidine-1-carboxylic acid [1-(4-ethoxy-phenyl)-piperidin-4-ylmethyl]-methyl-amide

HRID 511151
ノート
印刷プレビュー

反応式

HRID 511151 の反応式
ClC(Cl)(O[C:5](=[O:11])OC(Cl)(Cl)Cl)Cl.[CH3:13][NH:14][CH2:15][CH:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:27]=[CH:26][C:25](C(F)(F)F)=[CH:24][CH:23]=2)[CH2:18][CH2:17]1.C(N([CH2:37][CH3:38])CC)C.[N+:39]([C:42]1[CH:47]=[CH:46][C:45]([NH:48][CH:49]2[CH2:54][CH2:53][NH:52][CH2:51][CH2:50]2)=[CH:44][C:43]=1[C:55]([F:58])([F:57])[F:56])([O-:41])=[O:40].[OH2:59]>C(#N)C>[CH2:37]([O:59][C:25]1[CH:24]=[CH:23][C:22]([N:19]2[CH2:18][CH2:17][CH:16]([CH2:15][N:14]([CH3:13])[C:5]([N:52]3[CH2:51][CH2:50][CH:49]([NH:48][C:45]4[CH:46]=[CH:47][C:42]([N+:39]([O-:41])=[O:40])=[C:43]([C:55]([F:58])([F:56])[F:57])[CH:44]=4)[CH2:54][CH2:53]3)=[O:11])[CH2:21][CH2:20]2)=[CH:27][CH:26]=1)[CH3:38]
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 5

HCID 962WaterHCID 8471TriethylamineHCID 94429TriphosgeneHCID 43448257N-(4-Nitro-3-(trifluoromethyl)phenyl)piperidin-4-amineHCID 62648464Methyl-[1-(4-trifluoromethyl-phenyl)-piperidin-4-ylmethyl]-amine

生成物 1

HCID 58576857
4-(4-Nitro-3-trifluoromethyl-phenylamino)-piperidine-1-carboxylic acid [1-(4-ethoxy-phenyl)-piperidin-4-ylmethyl]-methyl-amide

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

Triphosgene (60 mg; 0.20 mmol) is added to a solution of methyl-[1-(4-trifluoromethyl-phenyl)-piperidin-4-ylmethyl]-amine (150 mg; 0.60 mmol) and triethylamine (185 μL; 1.33 mmol) in acetonitrile (6 mL). After stirring for 15 minutes a solution of (4-nitro-3-trifluoromethyl-phenyl)-piperidin-4-yl-amine (173 mg; 0.60 mmol, in acetonitrile (10 mL) is added. After 2 hours reaction time at room temperature, the mixture is poured into water (10 m) and the aqueous layer is extracted with ethyl acetate (3×50 mL). The combined organic layers are dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude product is purified by column chromatography on silica gel (Ethyl acetate:heptane 8:2) to afford the desired product (267 mg; 0.45 mmol). The structure was confirmed using Protocol II-E. Calculated mass=564; observed mass=564; HPLC retention time=7.73 min.

後処理

  1. customAfter 2 hours reaction time at room temperature
  2. extractionthe aqueous layer is extracted with ethyl acetate (3×50 mL)
  3. dry with materialThe combined organic layers are dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe crude product is purified by column chromatography on silica gel (Ethyl acetate:heptane 8:2)

出典と根拠

ORDレコード
ord-6e820a468081423999eb4ce5a2f5ffd6
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096524B2

反応ノート

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