Triethylamine → HCID 59853900, 화합물

HRID 2061234노트

반응식

HRID 2061234 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 59853900HCID 59853900, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-68b7d3d1572a47cfacc3d754e2780958
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08278329B2

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