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

反応式

HRID 1962366 の反応式
[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]

参加物

7

反応物 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

生成物 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

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e070a7aaa4b7451a82b4176890038241
出典データセット
uspto-grants-2013_04
特許番号
US08415369B2

関連ノート

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