Sodium Hydroxide → 2-butyl-3,5-dihydro-4H-imidazol-4-one

HRID 1452072

反応式

HRID 1452072 の反応式
Cl.C[O:3][C:4](=O)[CH2:5][NH2:6].[OH-].[Na+].CO[C:12](=[NH:17])[CH2:13][CH2:14][CH2:15][CH3:16]>CO.ClC1C=CC=CC=1>[CH2:13]([C:12]1[NH:17][C:4](=[O:3])[CH2:5][N:6]=1)[CH2:14][CH2:15][CH3:16]

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 122755Glycine methyl ester hydrochlorideHCID 5743466Methyl pentanimidate

生成物 1

HCID 109096542-butyl-3,5-dihydro-4H-imidazol-4-one

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 7964Chlorobenzene溶媒2 回

実験手順

31.71 g (0.25 mol) of glycine methyl ester hydrochloride was added to a solution of 10.1 g (0.25 mol) of sodium hydroxide in methanol at 0° C. After 15 minutes, 126.5 g of a 22.8 percent solution of pentanimidic acid methyl ester in chlorobenzene was instilled for 5 minutes to a white suspension. The light yellow suspension was stirred for 4 hours at room temperature and diluted with chlorobenzene (100 ml). The methanol was distilled off at a temperature of 26° C. and a pressure of 30 to 50 mbar, and the orange suspension was diluted with methylene chloride (100 ml) and then filtered. After removal of the solvent from the filtrate, 34.08 g (97 percent) of the title compound (content >95 percent, according to GC and 1H-NMR) was obtained.

後処理

  1. distillationThe methanol was distilled off at a temperature of 26° C.
  2. additiona pressure of 30 to 50 mbar, and the orange suspension was diluted with methylene chloride (100 ml)
  3. filtrationfiltered
  4. customAfter removal of the solvent from the filtrate

出典と根拠

ORDレコード
ord-8615f55fe1f44e9788d2026afdffc2f5
出典データセット
uspto-grants-1997_02
特許番号
US05606072

関連ノート

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