Hydrochloric Acid → HCID 20289969, 화합물

HRID 1856102노트

반응식

HRID 1856102 반응식
[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

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 20289954HCID 20289954, 화합물

생성물 1

HCID 20289969HCID 20289969, 화합물수율 104%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.).

후처리

  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.

출처 및 근거

ORD 기록
ord-4de323233b67494f9419979238fcab67
출처 데이터셋
uspto-grants-1980_08
특허 번호
US04218236

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