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 1619376ノート

反応式

HRID 1619376 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-8bcb5c8ae93f4cc6b702e5d4df988097
出典データセット
uspto-grants-2014_07
特許番号
US08772301B2

反応ノート

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