Triethylamine → HCID 86671304, 화합물

HRID 2367889

반응식

HRID 2367889 반응식
[CH3:1][N:2]([CH3:10])[N:3]1[CH2:8][CH2:7][C:6](=O)[CH2:5][CH2:4]1.C(N(CC)CC)C.Cl.[NH2:19][OH:20]>CO>[CH3:1][N:2]([CH3:10])[N:3]1[CH2:8][CH2:7][C:6](=[N:19][OH:20])[CH2:5][CH2:4]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 443297Hydroxyamine hydrochlorideHCID 567377821-(Dimethylamino)-4-piperidinone

생성물 1

HCID 86671304HCID 86671304, 화합물수율 68.3%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
37 °C

실험 절차

19.2 g 1-Dimethylamino-piperidin-4-one (prepared as described in Journal of Medicinal & Pharmaceutical Chemistry, 4, 423-36; 1961) and 30 g triethylamine are dissolved in 80 ml methanol. 18.8 g hydroxylamin hydrochloride is added in portions at ambient temperature. The internal temperature raises during the addition to 37° C. Then the mixture is heated to reflux for 3 hours, allowed to cool to room temperature, and then the solvent evaporated. The residue is partitioned between ethyl acetate and aqueous sodium bicarbonate. The organic layer is dried over sodium sulfate, and the solvent evaporated. Thus, 14.5 g 1-Dimethylamino-piperidin-4-one oxime is obtained. 1H-NMR (CDCl3): 8.10 ppm (s, broad, 1H), 2.75 ppm (m, 6H), 2.40 ppm (m, 2H), 2.40 ppm (s, 6H).

후처리

  1. temperatureThen the mixture is heated
  2. temperatureto reflux for 3 hours
  3. temperatureto cool to room temperature
  4. customthe solvent evaporated
  5. customThe residue is partitioned between ethyl acetate and aqueous sodium bicarbonate
  6. dry with materialThe organic layer is dried over sodium sulfate
  7. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-26a3a45656db442682014dd6ec817748
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703165B2

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