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

HRID 1648281ノート

反応式

HRID 1648281 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-732c333f4c1b424c99d169beb948e29f
出典データセット
uspto-grants-1995_07
特許番号
US05436240

反応ノート

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