2H-Azepine, 3,4,5,6-tetrahydro-7-methoxy- → 3-bromo-7,8,9,10-tetrahydropyrido[3',2':4,5]pyrimido[1,2-a]azepin-12(6H)-one

HRID 1619376노트

반응식

HRID 1619376 반응식
CO[C:3]1[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][N:9]=1.[NH2:10][C:11]1[C:12]([C:18](O)=[O:19])=[N:13][CH:14]=[C:15]([Br:17])[CH:16]=1>CN(C=O)C.O>[Br:17][C:15]1[CH:14]=[N:13][C:12]2[C:18](=[O:19])[N:9]3[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][C:3]3=[N:10][C:11]=2[CH:16]=1

참가 물질

5

반응물 2

HCID 756572H-Azepine, 3,4,5,6-tetrahydro-7-methoxy-HCID 497615813-Amino-5-bromopyridine-2-carboxylic acid

생성물 1

HCID 585742973-bromo-7,8,9,10-tetrahydropyrido[3',2':4,5]pyrimido[1,2-a]azepin-12(6H)-one

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A solution of 7-methoxy-3,4,5,6-tetrahydro-2H-azepine (1.0 g, 8.8 mmol) and 3-amino-5-bromopicolinic acid (1.9 g, 8.8 mmol) in DMF (70 mL) was stirred at 130° C. for 48 h. The reaction mixture was diluted with H2O (300 mL) and extracted with DCM (3×300 mL). The combined organic layers were washed with saturated sodium carbonate and brine, dried over Na2SO4. After filtration and concentration, the residue was purified by silica gel chromatography to give the desired product. MS (ESI):294, 296 (MH+).

후처리

  1. extractionextracted with DCM (3×300 mL)
  2. washThe combined organic layers were washed with saturated sodium carbonate and brine
  3. dry with materialdried over Na2SO4
  4. filtrationAfter filtration and concentration
  5. customthe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-8bcb5c8ae93f4cc6b702e5d4df988097
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772301B2

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