Hydrochloric Acid → HCID 23000985, 화합물

HRID 397742노트

반응식

HRID 397742 반응식
[CH2:1]([N:7]1[CH2:12][CH2:11][CH:10]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([NH:19]C(=O)C(O)(C)C)[CH:14]=2)[CH2:9][CH2:8]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].Cl>O1CCOCC1.O>[NH2:19][C:15]1[CH:14]=[C:13]([CH:10]2[CH2:11][CH2:12][N:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[CH2:8][CH2:9]2)[CH:18]=[CH:17][CH:16]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 23001068HCID 23001068, 화합물

생성물 1

HCID 23000985HCID 23000985, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

A solution of N-hexyl-4-(3-(2-hydroxy-2-methylpropanoylamino)phenyl)piperidine (Example 158) in 1,4-dioxan:5N aqueous hydrochloric acid solution (1:1, 10 ml) was heated under reflux overnight. The reaction mixture was cooled, diluted with water (10 ml) and extracted with diethyl ether (3×10 ml). The pH of the aqueous layer was adjusted to 8-9 using 5N aqueous sodium hydroxide, and extracted with dichloromethane (5×10 ml). The combined extracts were washed with brine (10 ml), dried (Na2SO4) and concentrated in vacuo to give the title compound as an oil which was not purified further (178 mg, 61% over two steps).

후처리

  1. temperatureunder reflux overnight
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with diethyl ether (3×10 ml)
  4. extractionextracted with dichloromethane (5×10 ml)
  5. washThe combined extracts were washed with brine (10 ml)
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5cba0c1961d44f6790a509783b3bd4b5
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610711B2

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