Ethyl Acetate → HCID 87214300、化合物

HRID 914790ノート

反応式

HRID 914790 の反応式
[F:1][C:2]1[C:10]([O:11][C:12]2[C:17]3=[C:18]([CH3:25])[C:19](C(O)(C)C)=[CH:20][N:16]3[N:15]=[CH:14][N:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([CH3:26])[NH:6]2.[C:27]([O-:30])([O-])=O.[K+].[K+].[C:33](OCC)(=[O:35])[CH3:34]>CN(C=O)C>[F:1][C:2]1[C:10]([O:11][C:12]2[C:17]3=[C:18]([CH3:25])[C:19]([O:35][CH2:33][C@@H:34]4[CH2:27][O:30]4)=[CH:20][N:16]3[N:15]=[CH:14][N:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([CH3:26])[NH:6]2

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 223379962-{4-[(4-Fluoro-2-methyl-1H-indol-5-yl)oxy]-5-methylpyrrolo[2,1-f][1,2,4]triazin-6-yl}propan-2-ol

生成物 1

HCID 87214300HCID 87214300、化合物収率 92%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of Example 1 (311 mg, 1 mmol), (2S)-(+)-glycidyl nosylate (311 mg, 1.2 mmol), and K2CO3 (200 mg, 1.45 mmol) in DMF (3 mL) was stirred at RT for 4 hr. The mixture was diluted with ethyl acetate and the solids were filtered. The filtrate was washed with brine, dried, and concentrated. The residue was purified by flash column chromatography (silica gel, 50% ethyl acetate in hexanes) to afford the title compound (340 mg, 92% yield). LC/MS; (M+H)+=369.1

後処理

  1. filtrationthe solids were filtered
  2. washThe filtrate was washed with brine
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by flash column chromatography (silica gel, 50% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-c8dedf8352aa4c2f91991e45493b68b3
出典データセット
uspto-grants-2007_09
特許番号
US07265113B2

反応ノート

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