Hydrochloric Acid → HCID 70043703, 화합물

HRID 2050569노트

반응식

HRID 2050569 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 520309Isobutyryl BromideHCID 20058556HCID 20058556, 화합물

생성물 1

HCID 70043703HCID 70043703, 화합물

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-f6854d385d7a421c9fe45aca0e300546
출처 데이터셋
uspto-grants-1991_05
특허 번호
US05013760

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