Triethylamine → 4-amino-N-(1-ethyl-piperidin-4-yl)-benzamide

HRID 1676525

反応式

HRID 1676525 の反応式
N1(O[C:11](=[O:19])[C:12]2[CH:17]=[CH:16][C:15]([NH2:18])=[CH:14][CH:13]=2)C2C=CC=CC=2N=N1.[NH2:20][CH:21]1[CH2:26][CH2:25][N:24]([CH2:27][CH3:28])[CH2:23][CH2:22]1.C(N(CC)CC)C>O1CCCC1>[NH2:18][C:15]1[CH:14]=[CH:13][C:12]([C:11]([NH:20][CH:21]2[CH2:26][CH2:25][N:24]([CH2:27][CH3:28])[CH2:23][CH2:22]2)=[O:19])=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 37349901-Ethylpiperidin-4-amineHCID 538445834-Amino-benzoic acid benzotriazol-1-yl ester

生成物 1

HCID 549158954-amino-N-(1-ethyl-piperidin-4-yl)-benzamide収率 84%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of 1.0424 g (4.1 mmole) of 4-amino-benzoic acid benzotriazol-1-yl ester and 8 mL of dry tetrahydrofuran at 0 degrees was added 0.5257 g (4.1 mmole) of 4-amino-1-ethylpiperidine followed by 1.0372 g (10.3 mmole) of triethylamine. The cooling bath was removed and the mixture stirred at room temperature for 65 minutes. Volatiles were removed under reduced pressure and the residue taken up in ethyl acetate, and the organic layer washed twice with 50 mL of 0.5 M sodium carbonate, 50 mL water, and then 50 mL brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 0.8522 g 4-amino-N-(1-ethyl-piperidin-4-yl)-benzamide, as a white solid which was used without further purification.

後処理

  1. customThe cooling bath was removed
  2. customVolatiles were removed under reduced pressure
  3. washthe organic layer washed twice with 50 mL of 0.5 M sodium carbonate, 50 mL water
  4. dry with material50 mL brine, dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-6618e55103764c5285ec53a92e237d85
出典データセット
uspto-grants-2011_08
特許番号
US08003785B2

関連ノート

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