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Water → 6-{4-[6-(4-Fluoro-phenyl)-2-(2-(R)-methyl-pyrrolidin-1-yl)-pyrimidin-4-yl]-3-(R)-methyl-piperazin-1-yl}-5-methyl-pyridine-2-carboxylic acid

HRID 2195065
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HRID 2195065 반응식
C[O:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH3:11])=[C:7]([N:12]2[CH2:17][CH2:16][N:15]([C:18]3[CH:23]=[C:22]([C:24]4[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=4)[N:21]=[C:20]([N:31]4[CH2:35][CH2:34][CH2:33][C@H:32]4[CH3:36])[N:19]=3)[C@H:14]([CH3:37])[CH2:13]2)[N:6]=1)=[O:4].O.O[Li].O>C1COCC1>[F:30][C:27]1[CH:26]=[CH:25][C:24]([C:22]2[N:21]=[C:20]([N:31]3[CH2:35][CH2:34][CH2:33][C@H:32]3[CH3:36])[N:19]=[C:18]([N:15]3[CH2:16][CH2:17][N:12]([C:7]4[N:6]=[C:5]([C:3]([OH:4])=[O:2])[CH:10]=[CH:9][C:8]=4[CH3:11])[CH2:13][C@H:14]3[CH3:37])[CH:23]=2)=[CH:29][CH:28]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 591683776-{4-[6-(4-Fluoro-phenyl)-2-(2-(R)-methyl-pyrrolidin-1-yl)-pyrimidin-4-yl]-3-(R)-methyl-piperazin-1-yl}-5-methyl-pyridine-2-carboxylic acid methyl ester

생성물 1

HCID 115622386-{4-[6-(4-Fluoro-phenyl)-2-(2-(R)-methyl-pyrrolidin-1-yl)-pyrimidin-4-yl]-3-(R)-methyl-piperazin-1-yl}-5-methyl-pyridine-2-carboxylic acid

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

반응 조건

온도
50 °C

실험 절차

To a solution of 6-{4-[6-(4-fluoro-phenyl)-2-(2-(R)-methyl-pyrrolidin-1-yl)-pyrimidin-4-yl]-3-(R)-methyl-piperazin-1-yl}-5-methyl-pyridine-2-carboxylic acid methyl ester (300 mg, 0.595 mmol) in THF, add water dropwise until the cloudiness almost persists. To this mixture add LiOH.H2O (50 mg, 1.2 mmol). Heat the mixture at 50° C. for 2 h, and then concentrate under reduced pressure. Add a small amount of water to the residue. Adjust the final pH to 6 and collect the off-white solid via filtration. Wash the solid with water and dry to afford the title compound.

후처리

  1. concentrationconcentrate under reduced pressure
  2. additionAdd a small amount of water to the residue
  3. customcollect the off-white solid
  4. filtrationvia filtration
  5. washWash the solid with water
  6. customdry

출처 및 근거

ORD 기록
ord-9038900300594125b792b0c266e4cd9d
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08334382B2

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