Hydrochloric Acid → HCID 20289969、化合物

HRID 1856102ノート

反応式

HRID 1856102 の反応式
[CH3:1][C:2]1[CH:26]=[CH:25][C:5]([O:6][CH:7]([C:9]2[S:13][C:12]([NH:14][C:15](=[O:24])[N:16]([CH2:18][CH:19](OC)[O:20]C)[CH3:17])=[N:11][N:10]=2)[CH3:8])=[CH:4][CH:3]=1.Cl>O>[CH3:1][C:2]1[CH:26]=[CH:25][C:5]([O:6][CH:7]([C:9]2[S:13][C:12]([N:14]3[CH:19]([OH:20])[CH2:18][N:16]([CH3:17])[C:15]3=[O:24])=[N:11][N:10]=2)[CH3:8])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 20289954HCID 20289954、化合物

生成物 1

HCID 20289969HCID 20289969、化合物収率 104%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture containing 3.5 grams of the 3-[5-[1-(4-methylphenoxy)ethyl]-1,3,4-thiadiazol-2-yl]-1-methyl-(2,2-dimethoxyethyl)urea (prepared above), 150 milliliters of water and 1.5 milliliters of concentrated hydrochloric acid (HCl) was refluxed for 25 minutes, then cooled with formation of an oil. The oil was extracted with chloroform, and the chloroform extract was dried over magnesium sulfate (MgSO4), filtered and topped on a roto-vac at 70° C. to yield 3.2 grams of an orange oil. It was dissolved in diethylether and heated with formation of crystals which were filtered off and dried in a vacuum oven at 70° C. to 1.8 grams of ivory crystals of [5-[1-(4-methylphenoxy)ethyl]-1,3,4-thiadiazol-2-yl]-1-methyl-4-hydroxy-2-imidazolidinone, (melting point 126°-128° C.).

後処理

  1. temperaturewas refluxed for 25 minutes
  2. temperaturecooled with formation of an oil
  3. extractionThe oil was extracted with chloroform
  4. extractionthe chloroform extract
  5. dry with materialwas dried over magnesium sulfate (MgSO4)
  6. filtrationfiltered
  7. customtopped on a roto-vac at 70° C.

出典と根拠

ORDレコード
ord-4de323233b67494f9419979238fcab67
出典データセット
uspto-grants-1980_08
特許番号
US04218236

反応ノート

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