Hydrochloric Acid → N-(2,3,6,7-tetrahydro-3-oxo-1H,5H-benzo(ij)quinolizin-2-yl)formamide

HRID 327438노트

반응식

HRID 327438 반응식
[OH-].[Na+].[O:3]=[C:4]1[C:13]([NH:19][CH:20]=[O:21])(C(OCC)=O)[CH2:12][C:11]2=[CH:22][CH:23]=[CH:24][C:9]3=[C:10]2[N:5]1[CH2:6][CH2:7][CH2:8]3.Cl>CO>[O:3]=[C:4]1[CH:13]([NH:19][CH:20]=[O:21])[CH2:12][C:11]2=[CH:22][CH:23]=[CH:24][C:9]3=[C:10]2[N:5]1[CH2:6][CH2:7][CH2:8]3

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86747427ethyl 2,3,6,7-tetrahydro-3-oxo-2-(formylamino)-1H,5H-benzo(ij)quinolizine-2-carboxylate

생성물 1

HCID 19919292N-(2,3,6,7-tetrahydro-3-oxo-1H,5H-benzo(ij)quinolizin-2-yl)formamide수율 104.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium hydroxide solution (5.0 mL of 4.0 N, 20 mmol) was slowly added to ethyl 2,3,6,7-tetrahydro-3-oxo-2-(formylamino)-1H,5H-benzo(ij)quinolizine-2-carboxylate (3.04 g, 10.0 mmol) in methanol (25 mL). After stirring at room temperature for 30 min, hydrochloric acid (5.0 mL of 4.0 N) was added and the precipitate was filtered off, washed with water and air dried to give 2.4 g of N-(2,3,6,7-tetrahydro-3-oxo-1H,5H-benzo(ij)quinolizin-2-yl)formamide, mp 149°-152° C. A portion of the product was recrystallized from ethyl acetate for analysis; mp 140°-143°. Anal. Calcd. for C13H14N2O2 : C, 67.81; H, 6.13; N, 12.17. Found: C, 67.67; H, 6.07; N, 11.94.

후처리

  1. filtrationthe precipitate was filtered off
  2. washwashed with water and air
  3. customdried

출처 및 근거

ORD 기록
ord-a7daa9475a134468afa5fac1ad7bec21
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05273975

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