Isobutylamine → HCID 58731015, 화합물

HRID 269563

반응식

HRID 269563 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][O:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][C:11]=2[C:20]2[C:21]([C:26]3[CH:31]=[C:30]([C:32]([O:34]C)=O)[CH:29]=[C:28]([C:36]([OH:38])=[O:37])[CH:27]=3)=[CH:22][CH:23]=[CH:24][CH:25]=2)=[CH:4][CH:3]=1.[CH3:39]N1CCOCC1.O.ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCC(N=C=N)C.[CH2:69]([NH2:73])[CH:70]([CH3:72])[CH3:71]>ClCCl.C(OCC)(=O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][O:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]([F:17])([F:19])[F:18])=[CH:12][C:11]=2[C:20]2[C:21]([C:26]3[CH:31]=[C:30]([C:32]([NH:73][CH2:69][CH:70]([CH3:72])[CH3:71])=[O:34])[CH:29]=[C:28]([C:36]([O:38][CH3:39])=[O:37])[CH:27]=3)=[CH:22][CH:23]=[CH:24][CH:25]=2)=[CH:4][CH:3]=1

참가 물질

8

반응물 5

HCID 6558IsobutylamineHCID 79724-MethylmorpholineHCID 27960291-Hydroxybenzotriazole hydrateHCID 219829211-(3-Dimethylaminopropyl)ethylcarbodiimide hydrochlorideHCID 58731014HCID 58731014, 화합물

생성물 1

HCID 58731015HCID 58731015, 화합물수율 51.8%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 2″-{[(4-fluorophenyl)methyl]oxy}-5-[(methyloxy)carbonyl]-5″-(trifluoromethyl)-1,1′:2′,1″-terphenyl-3-carboxylic acid (90 mg, 0.17 mmol), 4-methylmorpholine (34 mg, 45 μl, 0.34 mmol), 1-hydroxybenzotriazole hydrate (30 mg, 0.2 mmol), 1-(3-dimethylaminopropyl)-ethylcarbodiimide hydrochloride (38 mg, 0.2 mmol), and isobutylamine (25 mg, 34 ul, 0.34 mmol) in dichloromethane (3 ml) was stirred at room temperature for 2 hours. The mixture was diluted with ethyl acetate (10 ml), then washed with saturated NaHCO3, 2M HCl, water and brine. The organic phase was dried and evaporated. The residue was purified by chromatography in ethyl acetate/hexane (1:9-1:4) to give the title compound as a colourless solid (51 mg, 50%). LCMS: Rt=4.10 min. [M+H] 580

후처리

  1. washwashed with saturated NaHCO3, 2M HCl, water and brine
  2. customThe organic phase was dried
  3. customevaporated
  4. customThe residue was purified by chromatography in ethyl acetate/hexane (1:9-1:4)

출처 및 근거

ORD 기록
ord-4047a240d5c644808cfa34e5e1c68e3f
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07446222B2

연결된 노트

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