Diisopropyl Ether → HCID 13983449、化合物

HRID 580454ノート

反応式

HRID 580454 の反応式
[OH-].[K+].[O:3]1[CH2:8][CH2:7][N:6]([CH:9](O)[CH3:10])[CH2:5][CH2:4]1.[NH2:12][C:13]1[CH:22]=[CH:21][C:20]2[C:15](=[N:16][C:17](Cl)=[CH:18][CH:19]=2)[N:14]=1.C([O:27]C(C)C)(C)C>ClC1C=CC=CC=1.C(Cl)Cl.C(N(CCOCCOC)CCOCCOC)COCCOC>[NH2:12][C:13]1[CH:22]=[CH:21][C:20]2[C:15](=[N:16][C:17]([O:27][CH2:10][CH2:9][N:6]3[CH2:7][CH2:8][O:3][CH2:4][CH2:5]3)=[CH:18][CH:19]=2)[N:14]=1

参加物

8

反応物 4

HCID 7914Diisopropyl EtherHCID 14797Potassium HydroxideHCID 851997-Chloro-1,8-naphthyridin-2-amineHCID 30293761-Morpholinoethanol

生成物 1

HCID 13983449HCID 13983449、化合物

試薬・触媒・溶媒 3

HCID 112414Ethanamine, 2-(2-methoxyethoxy)-N,N-bis[2-(2-methoxyethoxy)ethyl]-触媒HCID 6344Dichloromethane溶媒HCID 7964Chlorobenzene溶媒

実験手順

Tris(3,6-dioxaheptyl)amine (1.47 g), pulverized potassium hydroxide (80% pure, 6.75 g) and morpholinoethanol (12 g) are added to a suspension of 2-amino-7-chloro-1,8-naphthyridine (16.2 g) in chlorobenzene (450 cc). The mixture is brought to 120° C. and maintained at this temperature for 3 hours. The suspension obtained after cooling is separated by filtration. The separated product is washed with chlorobenzene (3×50 cc) and water (3×50 cc). The solid obtained is redissolved in methylene chloride (400 cc). The insoluble material which remains is removed by filtration. The filtrate is dried over magnesium sulphate and concentrated to dryness at 40° C. under reduced pressure (4 kPa). The crude product obtained (23.5 g; m.p. 164° C.) is stirred in the presence of isopropyl ether (100 cc), filtered and dried at 30° C. under reduced pressure (0.07 kPa). 2-Amino-7-(2-morpholinoethoxy)-1,8-naphthyridine (13.9 g), m.p. 164° C., is obtained.

後処理

  1. customis brought to 120° C.
  2. temperaturemaintained at this temperature for 3 hours
  3. customThe suspension obtained
  4. temperatureafter cooling
  5. customis separated by filtration
  6. washThe separated product is washed with chlorobenzene (3×50 cc) and water (3×50 cc)
  7. customThe solid obtained
  8. customThe insoluble material which remains is removed by filtration
  9. dry with materialThe filtrate is dried over magnesium sulphate
  10. concentrationconcentrated to dryness at 40° C. under reduced pressure (4 kPa)
  11. customThe crude product obtained (23.5 g; m.p. 164° C.)
  12. filtrationfiltered
  13. customdried at 30° C. under reduced pressure (0.07 kPa)

出典と根拠

ORDレコード
ord-dbfe5bddf81c406cbadf904a890272a0
出典データセット
uspto-grants-1988_06
特許番号
US04753933

反応ノート

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