Hydrochloric Acid → HCID 20531187, 화합물

HRID 1759558노트

반응식

HRID 1759558 반응식
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]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 2781265HCID 2781265, 화합물HCID 20531188HCID 20531188, 화합물

생성물 1

HCID 20531187HCID 20531187, 화합물수율 86.7%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-130c7483f7234a46841a59ae1a09e3af
출처 데이터셋
uspto-grants-1982_07
특허 번호
US04341784

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