Potassium Hydroxide → 2-(2-Piperidin-4-ylphenyl)propan-2-ol

HRID 587637노트

반응식

HRID 587637 반응식
[OH:1][C:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[CH:11]1[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]1)([CH3:4])[CH3:3].[OH-].[K+]>C(O)(C)C.O>[NH:14]1[CH2:15][CH2:16][CH:11]([C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[C:2]([OH:1])([CH3:3])[CH3:4])[CH2:12][CH2:13]1

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 57459608Tert-butyl 4-[2-(1-hydroxy-1-methyl ethyl)phenyl]piperidine-1-carboxylate

생성물 1

HCID 574596102-(2-Piperidin-4-ylphenyl)propan-2-ol

시약·촉매·용매 2

HCID 962Water용매HCID 3776Isopropanol용매

실험 절차

A solution of intermediate D40 (27 g, 5.636 mmol) and KOH (2.433 g, 43.357 mmol) in isopropyl alcohol (13.5 ml) and water (27 ml) was heated at 180° C. under microwave irradiation for 60 min. After cooling to r.t., the mixture was washed with water and NaCl (aqueous saturated solution). The organic phase was dried (Na2SO4) and the solvent evaporated in vacuo. The crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 10% as eluent). The desired fractions were collected and concentrated in vacuo to yield intermediate compound D41 as a yellow solid (1.041. g, 84%). M.P. 219.5° C.

후처리

  1. washthe mixture was washed with water and NaCl (aqueous saturated solution)
  2. dry with materialThe organic phase was dried (Na2SO4)
  3. customthe solvent evaporated in vacuo
  4. customThe crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 10% as eluent)
  5. customThe desired fractions were collected
  6. concentrationconcentrated in vacuo
  7. customto yield intermediate compound D41 as a yellow solid (1.041. g, 84%)

출처 및 근거

ORD 기록
ord-fd7ad55c620c4796b71400d54d95b4ce
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09226930B2

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