Piperidine → HCID 69175643, 화합물

HRID 2237728노트

반응식

HRID 2237728 반응식
[CH3:1][O:2][C:3]1[CH:26]=[CH:25][C:6]([CH2:7][C@H:8]([CH:22]([CH3:24])[CH3:23])[CH2:9][C@H:10]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18])[C@@H:11]2[CH2:13][O:12]2)=[CH:5][C:4]=1[O:27][CH2:28][CH2:29][CH2:30][O:31][CH3:32].[NH:33]1[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]1>C(O)(C)C>[OH:12][C@H:11]([C@@H:10]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18])[CH2:9][C@H:8]([CH2:7][C:6]1[CH:25]=[CH:26][C:3]([O:2][CH3:1])=[C:4]([O:27][CH2:28][CH2:29][CH2:30][O:31][CH3:32])[CH:5]=1)[CH:22]([CH3:24])[CH3:23])[CH2:13][N:33]1[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]1

참가 물질

4

반응물 2

HCID 8082PiperidineHCID 59849018HCID 59849018, 화합물

생성물 1

HCID 69175643HCID 69175643, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A solution of 0.25 g of tert-butyl {3(S)-[4-methoxy-3-(3-methoxypropoxy)benzyl]-4-methyl-1(S)-(R)-oxiranylpentyl}carbamate in 4 ml of isopropanol and 0.99 ml of piperidine is stirred at 70° C. over 1 hour. The reaction mixture is concentrated by evaporation, and the residue is admixed with water and extracted with tert-butyl methyl ether (2×). The combined organic phases are washed with water and brine, dried over sodium sulphate and concentrated by evaporation. The title compound is obtained from the residue by means of flash chromatography (SiO2 60F) as a colourless oil. Rf=0.24 (9:1 dichloromethane-methanol); Rt=17.40 (gradient II).

후처리

  1. concentrationThe reaction mixture is concentrated by evaporation
  2. extractionextracted with tert-butyl methyl ether (2×)
  3. washThe combined organic phases are washed with water and brine
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-fa1eda9064144cb2bddb989d7000d9e5
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07718675B2

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