반응 #685027

ord-c2e866c8818e4e0d91f3499cf7eebf1d

반응 방정식

O=C(O)CCc1c[nH]c2c1C(=O)CCC2
3-Carboxyethyl-4-oxo-4,5,6,7-tetrahydro-1H-indole
O=S(=O)(O)O
sulfuric acid
CCO
ethanol
CCOC(=O)CCc1c[nH]c2c1C(=O)CCC2
3-(3-ethoxy-3-oxopropyl)-4-oxo-4,5,6,7-tetrahydro-1H-indole
수율 99.0%
CCOC(=O)CCc1c[nH]c2c1C(=O)CCC2
3-(3-Ethoxy-3-oxopropyl)-4-oxo-4,5,6,7-tetrahydro-1H-indole
수율 99.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was heated
  2. 2
    온도at reflux for 12 h
  3. 3
    농축The solution was concentrated under reduced pressure
  4. 4
    세척the resultant solids were washed with water (200 mL×2)
  5. 5
    기타The solids were air-dried

실험 절차

3-Carboxyethyl-4-oxo-4,5,6,7-tetrahydro-1H-indole (3, 52.0 g, 0.251 mol) in ethanol (100 mL) was added with sulfuric acid (1.0 mL). The reaction mixture was heated at reflux for 12 h. The solution was concentrated under reduced pressure and the resultant solids were washed with water (200 mL×2). The solids were air-dried to give 3-(3-ethoxy-3-oxopropyl)-4-oxo-4,5,6,7-tetrahydro-1H-indole (4, 59.0 g, 0.251 mol) as yellow solids in >99% yield.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07897602B2uspto-grants-2011_03