Tetrahydrofuran → Methyl-[1-(4-ethoxy-phenyl)-piperidin-4-ylmethyl]-amine

HRID 511150노트

반응식

HRID 511150 반응식
C(O[C:6](=O)[NH:7][CH2:8][CH:9]1[CH2:14][CH2:13][N:12]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH3:23])=[CH:17][CH:16]=2)[CH2:11][CH2:10]1)(C)(C)C.[H-].[Al+3].[Li+].[H-].[H-].[H-].O1CCCC1>O>[CH3:6][NH:7][CH2:8][CH:9]1[CH2:14][CH2:13][N:12]([C:15]2[CH:16]=[CH:17][C:18]([O:21][CH2:22][CH3:23])=[CH:19][CH:20]=2)[CH2:11][CH2:10]1

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 21226445Aluminium lithium hydrideHCID 58576345[1-(4-Ethoxy-phenyl)-piperidin-4-ylmethyl]-carbamic acid tert-butyl ester

생성물 1

HCID 58576685Methyl-[1-(4-ethoxy-phenyl)-piperidin-4-ylmethyl]-amine수율 98.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

[1-(4-Ethoxy-phenyl)-piperidin-4-ylmethyl]-carbamic acid tert-butyl ester (963 mg, 2.88 mmol, prepared in accordance with Example 106) is added to a molar solution of lithium aluminium hydride in tetrahydrofuran (10 mL, 10 mmol) and the resulting mixture is refluxed for 2 hours. After cooling with an ice bath, water (1 mL) is added carefully and the mixture is stirred overnight at room temperature. The reaction is then filtered and the filtrate is concentrated under reduced pressure. The residue obtained is dried under high vacuum to afford the desired product (701 mg; 2.83 mmol).

후처리

  1. temperaturethe resulting mixture is refluxed for 2 hours
  2. temperatureAfter cooling with an ice bath
  3. filtrationThe reaction is then filtered
  4. concentrationthe filtrate is concentrated under reduced pressure
  5. customThe residue obtained
  6. customis dried under high vacuum

출처 및 근거

ORD 기록
ord-4ad81030ba29402c833a23fd80857368
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096524B2

반응 노트

불러오는 중…