Triethylamine → HCID 66751353, 화합물

HRID 535016노트

반응식

HRID 535016 반응식
Cl.Cl.[C:3]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1)([CH3:6])([CH3:5])[CH3:4].[CH2:19]([O:26][C:27]1[CH:31]=[C:30]([C:32](O)=[O:33])[O:29][N:28]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(N(CC)CC)C.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1>CN(C)C=O.O>[CH2:19]([O:26][C:27]1[CH:31]=[C:30]([C:32]([N:16]2[CH2:17][CH2:18][N:13]([C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=3[C:3]([CH3:6])([CH3:4])[CH3:5])[CH2:14][CH2:15]2)=[O:33])[O:29][N:28]=1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1

참가 물질

8

반응물 5

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 136269673-(Benzyloxy)-1,2-oxazole-5-carboxylic acidHCID 667511491-(2-Tert-butylphenyl)piperazine dihydrochloride

생성물 1

HCID 66751353HCID 66751353, 화합물수율 73%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1-(2-tert-butylphenyl)piperazine dihydrochloride obtained in Reference Example 1 (2.1 g, 7.2 mmol), 3-(benzyloxy)isoxazole-5-carboxylic acid (1.58 g, 7.2 mmol), triethylamine (2.79 mL, 20.0 mmol), EDCI (1.92 g, 10.0 mmol) and HOBt (1.53 g, 10.0 mmol) in N,N-dimethylformamide (20 mL) was stirred at room temperature for 16 h. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to purify the residue by NH-silica gel column chromatography (hexane/ethyl acetate 90:10 to 50:50). Solvent was removed to obtain a solid (2.2 g, 73%).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customto purify the residue by NH-silica gel column chromatography (hexane/ethyl acetate 90:10 to 50:50)
  7. customSolvent was removed

출처 및 근거

ORD 기록
ord-3e075fcd244f4327a2b5ea86be14b52f
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853215B2

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