Diisopropyl Ether → HCID 13983449, 화합물

HRID 580454노트

반응식

HRID 580454 반응식
[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

참가 물질

8

반응물 4

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

생성물 1

HCID 13983449HCID 13983449, 화합물

시약·촉매·용매 3

HCID 112414Ethanamine, 2-(2-methoxyethoxy)-N,N-bis[2-(2-methoxyethoxy)ethyl]-촉매HCID 6344Dichloromethane용매HCID 7964Chlorobenzene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-dbfe5bddf81c406cbadf904a890272a0
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04753933

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