Acetic Anhydride → HCID 18328986, 화합물

HRID 1034256노트

반응식

HRID 1034256 반응식
[CH3:1][CH:2]1[C:14]2[NH:13][C:12]3[C:7](=[CH:8][C:9]([O:15][CH3:16])=[CH:10][CH:11]=3)[C:6]=2[CH2:5][CH2:4][NH:3]1.[C:17](OC(=O)C)(=[O:19])[CH3:18]>[NH4+].[OH-].C(OCC)(=O)C>[CH3:1][CH:2]1[C:14]2[NH:13][C:12]3[C:7](=[CH:8][C:9]([O:15][CH3:16])=[CH:10][CH:11]=3)[C:6]=2[CH2:5][CH2:4][N:3]1[C:17](=[O:19])[CH3:18]

참가 물질

5

반응물 2

HCID 7918Acetic AnhydrideHCID 710282,3,4,9-Tetrahydro-6-methoxy-1-methyl-1H-pyrido(3,4-b)indole

생성물 1

HCID 18328986HCID 18328986, 화합물

시약·촉매·용매 2

HCID 14923Ammonium Hydroxide촉매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 700 mg (3.24 mmol) 1-methyl-6-methoxy-1,2,3,4-tetrahydro-β-carboline, and 5 drops NH4OH in ethyl acetate was added 0.4 mL (3.88 mmol) acetic anhydride under N2 gas. The reaction was stirred for 20 min. and then washed with water. The organic layer collected was dried over MgSO4, filtered, and concentrated in vacuo to a dark oil. The oil was dissolved in methanol and chromatographed on reverse phase C-18 using methanol and water. The product was collected and concentrated to a white solid, which showed characteristic peaks: NMR (CDCl3) δ: 1.45 ppm (d, 3H), 2.25 ppm (s, 3H), 3.85 ppm (s, 3H).

후처리

  1. washwashed with water
  2. customThe organic layer collected
  3. dry with materialwas dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo to a dark oil
  6. dissolutionThe oil was dissolved in methanol
  7. customchromatographed on reverse phase C-18
  8. customThe product was collected
  9. concentrationconcentrated to a white solid, which

출처 및 근거

ORD 기록
ord-36e5f3b52127447b84cfc08d4bcd774f
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05314908

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