Water → HCID 18466731, 화합물

HRID 1601007노트

반응식

HRID 1601007 반응식
[CH:1]([C:4]1[C:13]([CH:14]([CH3:16])[CH3:15])=[N:12][C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[N:5]=1)([CH3:3])[CH3:2].[OH2:17]>C(O)(=O)C>[CH:1]([C:4]1[C:13]([CH:14]([CH3:16])[CH3:15])=[N:12][C:11]2[CH2:10][CH2:9][CH2:8][C:7](=[O:17])[C:6]=2[N:5]=1)([CH3:3])[CH3:2]

참가 물질

4

반응물 2

HCID 962Water2회HCID 18466650HCID 18466650, 화합물

생성물 1

HCID 18466731HCID 18466731, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

반응 조건

온도
80 °C

실험 절차

1.5 g of 5,6,7,8-tetrahydro-2,3-diisopropylquinoxaline was dissolved in 10 ml of acetic acid, followed by the dropwise addition of a solution of 1.0 g of chromic acid anhydride in acetic acid (6 ml)/water (1 ml). The obtained mixture was stirred at 80° C. for 2 hours, cooled by allowing to stand, and poured into water, followed by the extraction with ethyl acetate. The organic phase was washed with a saturated aqueous solution of sodium hydrogencarbonate and a saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate, and concentrated in a vacuum. The obtained residue was purified by silica gel chromatography (developer: 10% ethyl acetate/hexane) to give 0.6 g of the title compound as a brown solid.

후처리

  1. temperaturecooled
  2. extractionfollowed by the extraction with ethyl acetate
  3. washThe organic phase was washed with a saturated aqueous solution of sodium hydrogencarbonate
  4. dry with materiala saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate
  5. concentrationconcentrated in a vacuum
  6. customThe obtained residue was purified by silica gel chromatography (developer: 10% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-bb63f908d7c04a25b0cd3fb44f57e9c7
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05977125

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