Water → 2,2-Dimethyl-propionic acid 8-ethoxy-2-oxo-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-4-yl ester

HRID 1962366

반응식

HRID 1962366 반응식
[CH2:1]([O:3][N:4]1[CH2:24][CH2:23][C:7]2([NH:11][C:10](=[O:12])[C:9]([C:13]3[C:18]([CH3:19])=[CH:17][C:16]([CH3:20])=[CH:15][C:14]=3[CH3:21])=[C:8]2[OH:22])[CH2:6][CH2:5]1)[CH3:2].N1C=CC=CC=1.[C:31](Cl)(=[O:36])[C:32]([CH3:35])([CH3:34])[CH3:33].O>O1CCCC1.C(OCC)(=O)C>[CH2:1]([O:3][N:4]1[CH2:5][CH2:6][C:7]2([NH:11][C:10](=[O:12])[C:9]([C:13]3[C:18]([CH3:19])=[CH:17][C:16]([CH3:20])=[CH:15][C:14]=3[CH3:21])=[C:8]2[O:22][C:31](=[O:36])[C:32]([CH3:35])([CH3:34])[CH3:33])[CH2:23][CH2:24]1)[CH3:2]

참가 물질

7

반응물 4

HCID 962WaterHCID 1049PyridineHCID 62493Pivaloyl chlorideHCID 596145818-Ethoxy-4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-2-one

생성물 1

HCID 580312652,2-Dimethyl-propionic acid 8-ethoxy-2-oxo-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-4-yl ester

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

To 143 mg of 8-ethoxy-4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-2-one in 1 ml of tetrahydrofuran were added 36 μl of pyridine and 53 μl of pivaloyl chloride. After stirring at room temperature for 20 hours, water and ethyl acetate were added and the phases separated. The aqueous phase was extracted with ethyl acetate, the combined organic phases dried with sodium sulfate, filtered and concentrated. Chromatography (heptane/ethyl acetate 2:1) yielded 117 mg of 2,2-dimethyl-propionic acid 8-ethoxy-2-oxo-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-4-yl ester (title compound A54) as a solid, mp: 230-231° C.

후처리

  1. customthe phases separated
  2. extractionThe aqueous phase was extracted with ethyl acetate
  3. dry with materialthe combined organic phases dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e070a7aaa4b7451a82b4176890038241
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08415369B2

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