Methanol → 2,2-dimethylmalonic acid 5-{(4-carbamimidoylphenylamino)-[2-fluoro-3-(2-hydroxyethoxy)-5-metho xyphenyl]methyl}-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester 2,2-dimethylpropyl ester acetate

HRID 2089666

反応式

HRID 2089666 の反応式
[CH3:1][C:2]([CH3:59])([CH3:58])[CH2:3][O:4][C:5](=[O:57])[C:6]([CH3:56])([CH3:55])[C:7]([O:9][CH2:10][O:11][C:12]1[N:13]([C:49]2[N:54]=[CH:53][CH:52]=[CH:51][N:50]=2)[N:14]=[C:15]([CH:17]([NH:31][C:32]2[CH:37]=[CH:36][C:35]([C:38]([NH2:48])=[N:39]C(=O)C3C=CC=CC=3)=[CH:34][CH:33]=2)[C:18]2[CH:23]=[C:22]([O:24][CH3:25])[CH:21]=[C:20]([O:26][CH2:27][CH2:28][OH:29])[C:19]=2[F:30])[N:16]=1)=[O:8].CO>C(O)(=O)C>[C:5]([OH:57])(=[O:4])[CH3:6].[CH3:1][C:2]([CH3:59])([CH3:58])[CH2:3][O:4][C:5](=[O:57])[C:6]([CH3:56])([CH3:55])[C:7]([O:9][CH2:10][O:11][C:12]1[N:13]([C:49]2[N:50]=[CH:51][CH:52]=[CH:53][N:54]=2)[N:14]=[C:15]([CH:17]([NH:31][C:32]2[CH:33]=[CH:34][C:35]([C:38](=[NH:39])[NH2:48])=[CH:36][CH:37]=2)[C:18]2[CH:23]=[C:22]([O:24][CH3:25])[CH:21]=[C:20]([O:26][CH2:27][CH2:28][OH:29])[C:19]=2[F:30])[N:16]=1)=[O:8]

参加物

4

反応物 2

HCID 887MethanolHCID 682128732,2-dimethylmalonic acid 5-{(4-{amino[benzoylimino]methyl}phenylamino)-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]methyl}-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester 2,2-dimethylpropyl ester

生成物 1

HCID 866773942,2-dimethylmalonic acid 5-{(4-carbamimidoylphenylamino)-[2-fluoro-3-(2-hydroxyethoxy)-5-metho xyphenyl]methyl}-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester 2,2-dimethylpropyl ester acetate収率 181.9%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
40 °C

実験手順

To a mixture of 2,2-dimethylmalonic acid 5-{(4-{amino[benzoylimino]methyl}phenylamino)-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]methyl}-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester 2,2-dimethylpropyl ester (500 mg) and methanol (4 mL), acetic acid (1 mL) was added, and the resulting mixture was stirred at 40° C. for 4 hours. The mixture was concentrated under reduced pressure, and the residue obtained was purified by reverse phase silica gel column chromatography (mixed solvent of acetonitrile-water, containing 0.1% of acetic acid) to obtain the captioned compound (430 mg).

後処理

  1. additionwas added
  2. concentrationThe mixture was concentrated under reduced pressure
  3. customthe residue obtained
  4. customwas purified by reverse phase silica gel column chromatography (mixed solvent of acetonitrile-water, containing 0.1% of acetic acid)

出典と根拠

ORDレコード
ord-20b40d2bd81a4471912bb4b8601fd824
出典データセット
uspto-grants-2013_05
特許番号
US08436009B2

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