Hydrochloric Acid → HCID 70043703、化合物

HRID 2050569ノート

反応式

HRID 2050569 の反応式
[C:1](Br)(=[O:5])[CH:2]([CH3:4])[CH3:3].Br.Br.[C:9]1([CH2:15][CH2:16][NH:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][NH:24][CH2:25][CH2:26][C:27]2[CH:28]=[C:29]([OH:34])[C:30]([OH:33])=[CH:31][CH:32]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[ClH:35]>FC(F)(F)C(O)=O>[C:9]1([CH2:15][CH2:16][NH:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][NH:24][CH2:25][CH2:26][C:27]2[CH:28]=[C:29]([OH:34])[C:30]([OH:33])=[CH:31][CH:32]=2)[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1.[ClH:35].[ClH:35].[CH3:3][CH:2]([CH3:4])[C:1]([OH:5])=[O:33].[CH3:3][CH:2]([CH3:4])[C:1]([OH:5])=[O:33]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 520309Isobutyryl BromideHCID 20058556HCID 20058556、化合物

生成物 1

HCID 70043703HCID 70043703、化合物

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

Isobutyryl bromide (12 g) was added to a stirred solution of 4-[2-(6-(2-Phenylethylamino)hexylamino) ethyl]-1,2-benzenediol dihydrobromide (4 g) in trifluoracetic acid (100 ml). The solution was then stirred at room temperature for 24 hours. The excess solvent was evaporated and the residue treated with sodium bicarbonate solution. The basic mixture was thoroughly extracted with chloroform. The organic phase was separated, dried over magnesium sulfate, filtered and evaporated to leave a colorless oil which gave a white precipitate when treated with ethereal HCl. The white precipitate was recrystallised to give the title compound from ethanol as colorless prisms (2.8 g), m.p. 232°-234°.

後処理

  1. customThe excess solvent was evaporated
  2. additionthe residue treated with sodium bicarbonate solution
  3. extractionThe basic mixture was thoroughly extracted with chloroform
  4. customThe organic phase was separated
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customto leave a colorless oil which
  9. customgave a white precipitate when
  10. customThe white precipitate was recrystallised

出典と根拠

ORDレコード
ord-f6854d385d7a421c9fe45aca0e300546
出典データセット
uspto-grants-1991_05
特許番号
US05013760

反応ノート

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