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Triethylamine → 3-Ethoxycarbonyl-7,8-difluoro-1-methoxy-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine

HRID 1073596
ノート
印刷プレビュー

反応式

HRID 1073596 の反応式
C(N(CC)CC)C.Cl.[O:9]([NH2:11])[CH3:10].Cl[C:13]1[C:22]([C:23]([C:25](=[CH:31]N(C)C)[C:26]([O:28][CH2:29][CH3:30])=[O:27])=[O:24])=[CH:21][C:20]2[C:15](=[CH:16][C:17]([F:36])=[C:18]([F:35])[CH:19]=2)[N:14]=1>ClC(Cl)Cl>[CH2:29]([O:28][C:26]([C:25]1[C:23](=[O:24])[C:22]2[CH:21]=[C:20]3[CH:19]=[C:18]([F:35])[C:17]([F:36])=[CH:16][C:15]3=[N:14][C:13]=2[N:11]([O:9][CH3:10])[CH:31]=1)=[O:27])[CH3:30]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 53731972Ethyl 2-(2-chloro-6,7-difluoroquinoline-3-carbonyl)-3-dimethylaminoacrylate

生成物 1

HCID 148533423-Ethoxycarbonyl-7,8-difluoro-1-methoxy-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine収率 79.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
20 °C

実験手順

2.13 g of triethylamine are added to a suspension of 1.7 g of methoxylamine hydrochloride in 40 cm3 of trichloromethane. After stirring for 15 minutes at a temperature close to 20° C., 3.69 g of ethyl 2-(2-chloro-6,7-difluoroquinoline-3-carbonyl)-3-dimethylaminoacrylate are added to the solution obtained and the mixture is stirred for 4 hours and a half at about 20° C. The reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at a temperature close to 50° C. The residue is taken up in 70 cm3 of ethanol and 3.6 g of triethylamine and the mixture is heated for 30 minutes at a temperature close to 75° C. After cooling to about 20° C., the precipitate obtained is drained and washed with 3 times 30 cm3 of ethanol. 2.67 g of 3-ethoxycarbonyl-7,8-difluoro-1-methoxy-4-oxo-1,4-dihydro-benzo [b][1,8]naphthyridine are obtained in the form of a pale yellow solid melting at 266°-268° C.

後処理

  1. customclose to 20° C.
  2. customobtained
  3. stirringthe mixture is stirred for 4 hours
  4. customat about 20° C
  5. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at a temperature
  6. customclose to 50° C
  7. temperature3.6 g of triethylamine and the mixture is heated for 30 minutes at a temperature
  8. customclose to 75° C
  9. customthe precipitate obtained
  10. washwashed with 3 times 30 cm3 of ethanol

出典と根拠

ORDレコード
ord-cae6fe1a7e7040908a95edda2abd61ae
出典データセット
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04970213

反応ノート

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