Glyoxal → HCID 12918841、化合物

HRID 1155479ノート

反応式

HRID 1155479 の反応式
[CH3:1][C:2]([C:5]1[O:9][N:8]=[C:7]([NH:10][C:11]([NH:13][CH3:14])=[O:12])[CH:6]=1)([CH3:4])[CH3:3].[CH:15]([CH:17]=[O:18])=[O:16].[OH-].[Na+]>C(O)C>[CH3:4][C:2]([C:5]1[O:9][N:8]=[C:7]([N:10]2[CH:15]([OH:16])[CH:17]([OH:18])[N:13]([CH3:14])[C:11]2=[O:12])[CH:6]=1)([CH3:1])[CH3:3]

参加物

5

反応物 3

HCID 7860GlyoxalHCID 14798Sodium HydroxideHCID 186687Monoisouron

生成物 1

HCID 12918841HCID 12918841、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 2.0 grams (0.010 mole) of 1-[5-(1,1-dimethylethyl)-3-isoxazolyl]-3-methylurea in 50 milliliters of 95 percent ethanol was added 7.3 grams of a 40 percent aqueous glyoxal solution which had been previously adjusted to pH 7 with dilute sodium hydroxide solution. After standing at room temperature overnight, the solution was topped on a rotary evaporator to give an oily residue which was extracted with two 20 milliliter portions of chloroform. The extract was washed with saturated sodium chloride solution, filtered through silicone-treated paper, and concentrated on a rotary evaporator to give 2.0 grams of oily residue. Crystallization from ether gave 0.4 grams of white crystals of 3-[5-(1,1-dimethylethyl)-3-isoxazolyl]-4,5-dihydroxy-1-methyl-2-imidazolidinone, M.P. 153°-157° C., which had consistent mass, infrared and NMR spectra.

後処理

  1. customthe solution was topped on a rotary evaporator
  2. customto give an oily residue which
  3. extractionwas extracted with two 20 milliliter portions of chloroform
  4. washThe extract was washed with saturated sodium chloride solution
  5. filtrationfiltered through silicone-
  6. additiontreated paper
  7. concentrationconcentrated on a rotary evaporator

出典と根拠

ORDレコード
ord-226a0840e564419e92ffa3aaab41cb7d
出典データセット
uspto-grants-1981_11
特許番号
US04302239

反応ノート

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