Lithium hydroxide, monohydrate → 3-[3-(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R)-2-methyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-ureido]-propionic Acid

HRID 11630노트

반응식

HRID 11630 반응식
C[O:2][C:3](=[O:36])[CH2:4][CH2:5][NH:6][C:7]([NH:9][C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:11]=1[O:17][CH2:18][C:19]([N:21]1[CH2:26][CH2:25][N:24]([CH2:27][C:28]2[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=2)[CH2:23][C@H:22]1[CH3:35])=[O:20])=[O:8].O.[OH-].[Li+]>O1CCCC1.CO.O>[Cl:16][C:14]1[CH:13]=[CH:12][C:11]([O:17][CH2:18][C:19]([N:21]2[CH2:26][CH2:25][N:24]([CH2:27][C:28]3[CH:29]=[CH:30][C:31]([F:34])=[CH:32][CH:33]=3)[CH2:23][C@H:22]2[CH3:35])=[O:20])=[C:10]([NH:9][C:7](=[O:8])[NH:6][CH2:5][CH2:4][C:3]([OH:36])=[O:2])[CH:15]=1

참가 물질

6

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 696553713-[3-(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R)-2-methyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-ureido]-propionic Acid Methyl Ester

생성물 1

HCID 210436923-[3-(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R)-2-methyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-ureido]-propionic Acid

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 3-[3-(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R)-2-methyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-ureido]-propionic acid methyl ester (0.057 g, 0.11 mmol) in tetrahydrofuran (3 mL), methanol (3 mL) and water (1 mL) was added lithium hydroxide monohydrate (0.023 g, 0.55 mmol). The reaction was stirred at ambient temperature overnight, concentrated in vacuo, taken up in methanol, passed through an ion exchange column and then treated with hydrogen chloride gas to give the title compound as its hydrochloride salt (0.035 g, LRMS: 507.2).

후처리

  1. concentrationconcentrated in vacuo
  2. additiontreated with hydrogen chloride gas

출처 및 근거

ORD 기록
ord-f75693f6867e4644b7b4bb511c63c3fc
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098212B2

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