Hydrochloric Acid → HCID 19439052, 화합물

HRID 1920751노트

반응식

HRID 1920751 반응식
[OH-].[Na+].C([O:5][C:6](=[O:18])[CH2:7][CH:8]1[CH2:13][CH2:12][N:11]([C:14]([CH3:17])([CH3:16])[CH3:15])[CH2:10][CH2:9]1)C.Cl>O.C(O)C>[C:14]([N:11]1[CH2:10][CH2:9][CH:8]([CH2:7][C:6]([OH:18])=[O:5])[CH2:13][CH2:12]1)([CH3:17])([CH3:15])[CH3:16]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57733330HCID 57733330, 화합물

생성물 1

HCID 19439052HCID 19439052, 화합물수율 19.7%

시약·촉매·용매 1

HCID 19096565Water ethanol용매

실험 절차

To a solution of NaOH in water/ethanol (v/v=40/10, 50 mL) (1-tert-butyl-piperidin-4-yl)-acetic acid ethyl ester (4.03 g, 17.8 mmol) was added and the mixture was stirred at r.t. overnight. 1 N aq. HCl was added to adjust the pH to 5. Volotiles were evaporated in vacuo, the residue was diluted with methanol (30 mL), and the insoluble inorganic salts were removed by filtration. The filtrate was concentrated and purified by column chromatography on silica gel (CH2Cl2/MeOH=20/1 to 5/1) to give 0.7 g of title compound as a light grey powder. 1H NMR (400 MHz, DMSO-d6): 3.15-3.08 (br m, 2H), 2.30 (br t, J=11.2 Hz, 2H), 2.05 (d, J=6.4 Hz, 2H), 1.71-1.68 (m, 3H), 1.30-1.27 (m, 2H), 1.10 (s, 9H).

후처리

  1. customVolotiles were evaporated in vacuo
  2. additionthe residue was diluted with methanol (30 mL)
  3. customthe insoluble inorganic salts were removed by filtration
  4. concentrationThe filtrate was concentrated
  5. custompurified by column chromatography on silica gel (CH2Cl2/MeOH=20/1 to 5/1)

출처 및 근거

ORD 기록
ord-40771122922846a89c7a0486c0cb24c2
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08173639B2

반응 노트

불러오는 중…