Acetic Anhydride → HCID 18328986、化合物

HRID 1034256ノート

反応式

HRID 1034256 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 18328986HCID 18328986、化合物

試薬・触媒・溶媒 2

HCID 14923Ammonium Hydroxide触媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-36e5f3b52127447b84cfc08d4bcd774f
出典データセット
uspto-grants-1994_05
特許番号
US05314908

反応ノート

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