Triethylamine → HCID 59853900、化合物

HRID 2236014ノート

反応式

HRID 2236014 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([N:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[CH2:11][CH2:10][C:9]3[CH:18]=[CH:19][CH:20]=[CH:21][C:8]2=3)[CH2:3][CH2:2]1.[C:22]([NH:26][C:27](=[O:33])[CH2:28][CH2:29][C:30](O)=[O:31])([CH3:25])([CH3:24])[CH3:23].Cl.C(N=C=NCCCN(C)C)C.C(N(CC)CC)C>ClCCl.CN(C)C1C=CN=CC=1>[C:22]([NH:26][C:27](=[O:33])[CH2:28][CH2:29][C:30]([N:1]1[CH2:6][CH2:5][CH:4]([N:7]2[C:8]3[CH:21]=[CH:20][CH:19]=[CH:18][C:9]=3[CH2:10][CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]2=3)[CH2:3][CH2:2]1)=[O:31])([CH3:25])([CH3:23])[CH3:24]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 2450094-(tert-Butylamino)-4-oxobutanoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 68422590HCID 68422590、化合物

生成物 1

HCID 59853900HCID 59853900、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

83.2 mg (0.299 mmol) of 5-(4-piperidinyl)-10,11-dihydro-5H-dibenzo[b,f]azepine, 62.2 mg (0.359 mmol) of 4-(t-butylamino)-4-oxobutanoic acid and 82.6 mg (0.431 mmol) of 1-ethyl-3-(3′-dimethylaminopropyl)carbodiimide hydrochloride were dissolved in 5 ml of dichloromethane. 0.06 ml (0.431 mmol) of triethylamine and 3.67 mg (0.03 mmol) of 4-dimethylaminopyridine were added to the obtained solution, and they were stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure. Ethyl acetate was added thereto. After washing with 1 N aqueous hydrochloric acid solution, the organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by the silica gel chromatography (dichloromethane: methanol=9:1) to obtain the title compound.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionEthyl acetate was added
  3. washAfter washing with 1 N aqueous hydrochloric acid solution
  4. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by the silica gel chromatography (dichloromethane: methanol=9:1)

出典と根拠

ORDレコード
ord-d3c01b4fa5c443c7bcfa2c1ec76fe836
出典データセット
uspto-grants-2010_05
特許番号
US07713957B2

反応ノート

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