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Triethylamine → HCID 86606825, 화합물

HRID 1437674
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HRID 1437674 반응식
[CH2:1]([C@H:8]1[C@@H:13]([O:14][CH2:15][C:16]2[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[C:18]([C:26]([F:29])([F:28])[F:27])[CH:17]=2)[CH2:12][CH2:11][NH:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[CH2:31]([N:33]([CH2:39][CH3:40])[CH2:34][CH2:35][C:36](O)=[O:37])[CH3:32].CCN(CC)CC.CCN=C=NCCCN(C)C.Cl>CN(C=O)C.O>[CH2:1]([C@H:8]1[C@@H:13]([O:14][CH2:15][C:16]2[CH:17]=[C:18]([C:26]([F:29])([F:27])[F:28])[CH:19]=[C:20]([C:22]([F:23])([F:24])[F:25])[CH:21]=2)[CH2:12][CH2:11][N:10]([C:36](=[O:37])[CH2:35][CH2:34][N:33]([CH2:39][CH3:40])[CH2:31][CH3:32])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 3084241N,N-diethyl-beta-alanine hydrochlorideHCID 86606823HCID 86606823, 화합물

생성물 1

HCID 86606825HCID 86606825, 화합물수율 42,767.102%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6228Dimethylformamide용매

실험 절차

To a solution of the compound (0.15 g) obtained in Example 404, 3-diethylaminopropionic acid hydrochloride (0.078 mg), Et3N (0.150 ml) and HoBt.H2O (0.083 mg) in DMF (2 ml), WSC.HCl (0.138 mg) was added, and the reaction mixture was stirred at room temperature for 12 hours. The reaction mixture was concentrated under reduced pressure, and then the residue was dissolved in ethyl acetate. The organic layer was washed with an aqueous saturated sodium bicarbonate solution and brine, dried, and then the solvent was evaporated under reduced pressure. The obtained residue was purified by preparative thin layer chromatography to obtain the title compound as pale yellow oil (0.100 g, 51%).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe organic layer was washed with an aqueous saturated sodium bicarbonate solution and brine
  4. customdried
  5. customthe solvent was evaporated under reduced pressure
  6. customThe obtained residue was purified by preparative thin layer chromatography

출처 및 근거

ORD 기록
ord-053f4c9f343842b0a4b7b6191a51a64f
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07622487B2

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