Lithium Hydroxide → 3-[4-(2-tert-Butyl-6-cyclopropyl-pyrimidin-4-yl)-piperazin-1-yl]-propan-1-ol

HRID 219712노트

반응식

HRID 219712 반응식
[C:1]([C:5]1[N:10]=[C:9]([N:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][CH2:19][O:20]C(=O)C)[CH2:13][CH2:12]2)[CH:8]=[C:7]([CH:24]2[CH2:26][CH2:25]2)[N:6]=1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Li+]>O1CCCC1.O>[C:1]([C:5]1[N:10]=[C:9]([N:11]2[CH2:12][CH2:13][N:14]([CH2:17][CH2:18][CH2:19][OH:20])[CH2:15][CH2:16]2)[CH:8]=[C:7]([CH:24]2[CH2:26][CH2:25]2)[N:6]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 69026905Acetic acid 3-[4-(2-tert-butyl-6-cyclopropyl-pyrimidin-4-yl)-piperazin-1-yl]-propyl ester

생성물 1

HCID 690296093-[4-(2-tert-Butyl-6-cyclopropyl-pyrimidin-4-yl)-piperazin-1-yl]-propan-1-ol수율 30.8%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

3.7 g of acetic acid 3-[4-(2-tert-butyl-6-cyclopropyl-pyrimidin-4-yl)-piperazin-1-yl]-propyl ester (10.2 mmol) and 0.4 g of lithium hydroxide (16.7 mmol) were stirred overnight in 20 ml of tetrahydrofuran and 20 ml of water. The reaction mixture was partitioned between water and ethyl acetate. The organic layer was dried over magnesium sulfate, filtered, and the solvent was evaporated. The crude product was purified by chromatography on silica gel using dichloromethane-methanol (0-8%) as eluent to yield 1.0 g of the title compound.

후처리

  1. customThe reaction mixture was partitioned between water and ethyl acetate
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. filtrationfiltered
  4. customthe solvent was evaporated
  5. customThe crude product was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-57f645df30404330a82ef0f3e30272c0
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202868B2

반응 노트

불러오는 중…