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

HRID 868592ノート

反応式

HRID 868592 の反応式
[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

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 256005n-methylhydrazinecarboxamideHCID 516892Sodium BicarbonateHCID 13934409HCID 13934409、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-175587cf0d0d4bb58142fc32a646438f
出典データセット
uspto-grants-1988_10
特許番号
US04780477

反応ノート

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