Isobutylamine → HCID 58731015、化合物

HRID 269563

反応式

HRID 269563 の反応式
[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

参加物

8

反応物 5

HCID 6558IsobutylamineHCID 79724-MethylmorpholineHCID 27960291-Hydroxybenzotriazole hydrateHCID 219829211-(3-Dimethylaminopropyl)ethylcarbodiimide hydrochlorideHCID 58731014HCID 58731014、化合物

生成物 1

HCID 58731015HCID 58731015、化合物収率 51.8%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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

後処理

  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)

出典と根拠

ORDレコード
ord-4047a240d5c644808cfa34e5e1c68e3f
出典データセット
uspto-grants-2008_11
特許番号
US07446222B2

関連ノート

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