Hydrochloric Acid → HCID 20531187、化合物

HRID 1759558ノート

反応式

HRID 1759558 の反応式
Cl[C:2]1[N:11]=[C:10]2[C:5]([C:6](=[O:19])[C:7]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:8][N:9]2[CH2:12][CH3:13])=[CH:4][C:3]=1[F:20].[C:21]([CH2:24][NH:25][CH:26]1[CH2:30][CH2:29][NH:28][CH2:27]1)(=[O:23])[CH3:22].C(N(CC)CC)C.Cl>C(Cl)(Cl)Cl>[C:21]([CH2:24][NH:25][CH:26]1[CH2:30][CH2:29][N:28]([C:2]2[N:11]=[C:10]3[C:5]([C:6](=[O:19])[C:7]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:8][N:9]3[CH2:12][CH3:13])=[CH:4][C:3]=2[F:20])[CH2:27]1)(=[O:23])[CH3:22]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 2781265HCID 2781265、化合物HCID 20531188HCID 20531188、化合物

生成物 1

HCID 20531187HCID 20531187、化合物収率 86.7%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A mixture containing ethyl 7-chloro-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylate (2.99 g), 3-(N-acetylmethylamino)pyrrolidine (2.13 g), triethylamine (1.52 g), and chloroform (30 ml) was heated to reflux for 4 hours with stirring. After cooling the mixture, 5% hydrochloric acid (20 ml) was added with stirring. The chloroform layer was separated off and the solvent was evaporated. To the residue was added 20 ml of acetonitrile and the mixture was cooled. The resulting precipitate was collected and recrystallized from acetonitrile to give 3.51 g of ethyl 7-[3-(N-acetylmethylamino)-1-pyrrolidinyl]-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylate, m.p. 212°-213° C.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 4 hours
  3. additionwas added
  4. stirringwith stirring
  5. customThe chloroform layer was separated off
  6. customthe solvent was evaporated
  7. additionTo the residue was added 20 ml of acetonitrile
  8. temperaturethe mixture was cooled
  9. customThe resulting precipitate was collected
  10. customrecrystallized from acetonitrile

出典と根拠

ORDレコード
ord-130c7483f7234a46841a59ae1a09e3af
出典データセット
uspto-grants-1982_07
特許番号
US04341784

反応ノート

読み込み中…