Hydrochloric Acid → HCID 70549035、化合物

HRID 1680182ノート

反応式

HRID 1680182 の反応式
[C:1]12([NH:12][C:13](=[O:26])[CH2:14][N:15]3C(=O)C4=CC=CC=C4C3=O)[CH2:10][CH:6]([CH2:7][CH2:8][CH2:9]1)[CH:5]1[CH2:11][CH:2]2[CH2:3][CH2:4]1.O.NN.C(O)C.[ClH:33]>C1C=CC=CC=1>[ClH:33].[C:1]12([NH:12][C:13](=[O:26])[CH2:14][NH2:15])[CH2:10][CH:6]([CH2:7][CH2:8][CH2:9]1)[CH:5]1[CH2:11][CH:2]2[CH2:3][CH2:4]1

参加物

6

反応物 4

HCID 313Hydrochloric Acid2 回HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)HCID 54401911HCID 54401911、化合物

生成物 1

HCID 70549035HCID 70549035、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 1.39 g (3.94 millimoles) of N-(1-tricyclo[4.3.1.12,5 ]undecyl)-2-phthalimidoacetamide, 0.30 g (4.37 millimoles) of 80% hydrazine hydrate and 10 ml of ethanol was refluxed under agitation for 4 hours. The reaction temperature was lowered to 60° C., and 5 ml of 10% hydrochloric acid was added and the mixture was agitated for 2 hours. After cooling, the precipitate was recovered by filtration, and the pH of the filtrate was adjusted to 9 with a 5% aqueous solution of sodium hydroxide and the mixture was extracted with diethyl ether. The diethyl ether solution was condensed, and the residue was dissolved in 20 ml of dry benzene and dry hydrogen chloride gas was blown into the solution. The formed white precipitate was recovered by filtration and recrystallized from ethanolacetone to obtain 0.59 g (the yield being 58%) of the intended compound having a melting point of 225° to 229° C.

後処理

  1. temperaturewas refluxed under agitation for 4 hours
  2. customwas lowered to 60° C.
  3. temperatureAfter cooling
  4. filtrationthe precipitate was recovered by filtration
  5. extractionthe mixture was extracted with diethyl ether
  6. customcondensed
  7. filtrationThe formed white precipitate was recovered by filtration
  8. customrecrystallized from ethanolacetone
  9. customto obtain 0.59 g (the yield

出典と根拠

ORDレコード
ord-1b2920c4266046638fb931d6ce6ac9c3
出典データセット
uspto-grants-1981_06
特許番号
US04272536

反応ノート

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