Triethylamine → HCID 15232832, 화합물

HRID 1110223

반응식

HRID 1110223 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([NH2:11])[CH:10]=1)[C:5]([OH:7])=[O:6].C(N([CH2:17][CH3:18])CC)C.[C:19](Cl)(=[O:29])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]>C(Cl)Cl.C1COCC1>[O:29]=[C:19]([NH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([NH:11][C:19](=[O:29])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:17][CH3:18])[CH:10]=1)[C:5]([OH:7])=[O:6])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 120623,5-Diaminobenzoic acidHCID 66982Decanoyl chloride

생성물 1

HCID 15232832HCID 15232832, 화합물수율 57%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of 5 g (0.033 mol) of 3,5-diaminobenzoic acid in 100 ml of methylene chloride, 50 ml of THF and 18 ml (0.13 mol) of triethylamine stirred at room temperature was added 17 ml (0.08 mol) of decanoyl chloride dropwise over 10 minutes. The reaction mixture was stirred for 18 hours, filtered and the filtrate was concentrated at reduced pressure. Water was added to the residue and the product was extracted with ethyl acetate. The dried extract was concentrated at reduced pressure and the solid residue was recrystallized twice from methanol-water to give 8.6 g (57% yield, mp 208°-209°) of 3,5-bis[(1-oxodecyl)amino]benzoic acid.

후처리

  1. stirringThe reaction mixture was stirred for 18 hours
  2. filtrationfiltered
  3. concentrationthe filtrate was concentrated at reduced pressure
  4. additionWater was added to the residue
  5. extractionthe product was extracted with ethyl acetate
  6. extractionThe dried extract
  7. concentrationwas concentrated at reduced pressure
  8. customthe solid residue was recrystallized twice from methanol-water

출처 및 근거

ORD 기록
ord-58c55d9bc8974d7a9e45d80feff3f1d4
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05324747

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