Triethylamine → HCID 15232832、化合物

HRID 1110223

反応式

HRID 1110223 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 15232832HCID 15232832、化合物収率 57%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-58c55d9bc8974d7a9e45d80feff3f1d4
出典データセット
uspto-grants-1994_06
特許番号
US05324747

関連ノート

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