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

HRID 1648281노트

반응식

HRID 1648281 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- (formyl amino) - 1H,5 H-benzo(ij )quinolizine-2-carboxyl ate (3.134 g, 10.0 mmol) in methanol (25 mL). After stirring at room temperature for 30 rain, 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. Calc'd for C13H14N2O2 : C, 67.81; H, 6.13; N, 12.17. Found: C, 67.67; H, 6.07; N, 11.94.

후처리

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

출처 및 근거

ORD 기록
ord-732c333f4c1b424c99d169beb948e29f
출처 데이터셋
uspto-grants-1995_07
특허 번호
US05436240

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