Water → Ethyl (3-oxo-1-phenyl-1,4-diazaspiro[5.5]undec-4-yl)acetate

HRID 1894861ノート

反応式

HRID 1894861 の反応式
C(=O)([O-])[O-].[K+].[K+].[C:7]1([NH:13][C:14]2([CH2:20][NH:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.Cl[CH2:29][C:30](Cl)=[O:31].O>CN(C)C=O>[O:31]=[C:30]1[N:21]([CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH2:20][C:14]2([CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[N:13]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH2:29]1

参加物

6

反応物 4

HCID 962WaterHCID 6577Chloroacetyl chlorideHCID 11430Potassium CarbonateHCID 86646976Ethyl [(1-phenylaminocyclohexylmethyl)amino]acetate

生成物 1

HCID 86646979Ethyl (3-oxo-1-phenyl-1,4-diazaspiro[5.5]undec-4-yl)acetate収率 97%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

95 mg (0.69 mmol) of potassium carbonate are added to a solution of 200 mg (0.69 mmol) of ethyl [(1-phenylaminocyclohexylmethyl)amino]-acetate and 55 μl (0.69 mmol) of chloroacetyl chloride in 15 ml of dimethylformamide. The reaction medium is stirred at reflux for 6 h and poured into water and extracted with ethyl acetate. The organic phases are collected and washed with water. They are dried over sodium sulfate. The solvents are evaporated. 220 mg of ethyl (3-oxo-1-phenyl-1,4-diazaspiro[5.5]undec-4-yl)acetate are obtained in the form of an orange oil. Yield=97%.

後処理

  1. temperatureat reflux for 6 h
  2. extractionextracted with ethyl acetate
  3. customThe organic phases are collected
  4. washwashed with water
  5. dry with materialThey are dried over sodium sulfate
  6. customThe solvents are evaporated

出典と根拠

ORDレコード
ord-4f23c8d1401142da94dce7892fd7b8ba
出典データセット
uspto-grants-2013_08
特許番号
US08513307B2

反応ノート

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