Hydrochloric Acid → 1-[(E)-[1-[2-[di(propan-2-yl)amino]ethyl]-5-methyl-2-oxoindol-3-ylidene]amino]-3-methylurea

HRID 868592노트

반응식

HRID 868592 반응식
[CH:1]([N:4]([CH:19]([CH3:21])[CH3:20])[CH2:5][CH2:6][N:7]1[C:17]2[C:12](=[CH:13][C:14]([CH3:18])=[CH:15][CH:16]=2)[C:10](=O)[C:8]1=[O:9])([CH3:3])[CH3:2].[CH3:22][NH:23][C:24](=[O:27])[NH:25][NH2:26].Cl.C(=O)(O)[O-].[Na+]>O.C(O)C>[CH3:22][NH:23][C:24](=[O:27])[NH:25]/[N:26]=[C:10]1/[C:8](=[O:9])[N:7]([CH2:6][CH2:5][N:4]([CH:19]([CH3:21])[CH3:20])[CH:1]([CH3:3])[CH3:2])[C:17]2[C:12]/1=[CH:13][C:14]([CH3:18])=[CH:15][CH:16]=2

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 256005n-methylhydrazinecarboxamideHCID 516892Sodium BicarbonateHCID 13934409HCID 13934409, 화합물

생성물 1

HCID 1784859471-[(E)-[1-[2-[di(propan-2-yl)amino]ethyl]-5-methyl-2-oxoindol-3-ylidene]amino]-3-methylurea수율 61.8%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a solution of 1.00 g of 1-(2-diisopropylaminoethyl)-5-methylisatin and 0.34 g of 4-methylsemicarbazide in 15 ml of a mixture of ethanol and water (2:1) was added 3.8 ml of a 1N-hydrochloric acid. The mixture was stirred for 16 hours at room temperature. To the reaction mixture was added an aqueous sodium bicarbonate solution, and the mixture was extracted with chloroform. The chloroform layer was washed with water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was recrystallized from ethanol to obtain 0.77 g of (E)-1-(2-diisopropylaminoethyl)-5-methylisatin 3-(4-methylsemicarbazone) having a melting point of 157.5°-158.5° C.

후처리

  1. extractionthe mixture was extracted with chloroform
  2. washThe chloroform layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-175587cf0d0d4bb58142fc32a646438f
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04780477

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