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

반응식

HRID 2089666 반응식
[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]

참가 물질

4

반응물 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

생성물 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 acetate수율 181.9%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
40 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-20b40d2bd81a4471912bb4b8601fd824
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08436009B2

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