Hydrochloric Acid → HCID 44229381、化合物

HRID 1951306ノート

反応式

HRID 1951306 の反応式
Cl.[O:2]=[C:3]1[N:12]([CH2:13][CH2:14][CH2:15][N:16]([CH2:20][CH2:21][CH2:22][CH2:23][NH:24][CH2:25][CH2:26][CH2:27][N:28]2[C:37](=[O:38])[C:36]3[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=3)[NH:30][C:29]2=[O:39])[C:17](=[O:19])[CH3:18])[C:11](=[O:40])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[NH:4]1.[CH2:41](N(CC)CC)C.C=O.[BH4-].[Na+]>ClCCl.CO>[O:2]=[C:3]1[N:12]([CH2:13][CH2:14][CH2:15][N:16]([CH2:20][CH2:21][CH2:22][CH2:23][N:24]([CH2:25][CH2:26][CH2:27][N:28]2[C:37](=[O:38])[C:36]3[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=3)[NH:30][C:29]2=[O:39])[CH3:41])[C:17](=[O:19])[CH3:18])[C:11](=[O:40])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[NH:4]1

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 8471TriethylamineHCID 4311764Sodium borohydrideHCID 44229378Remogliflozin etabonate

生成物 1

HCID 44229381HCID 44229381、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

Hydrochloride acid salt of N-[3-(2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)propyl]-N-{4-[3-(2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)propylamino]butyl}acetamide (2 g, 3.5 mmol was dissolved in 80 mL dichloromethane and 10 mL, methanol. Triethylamine (0.45 g, 4.5 mmol) and paraformaldehyde (0.14 g, 4.5 mmol) was added thereto and stirred for 2 hours at room temperature. After concentration of the solvent, 40 mL methanol and sodium borohydride (0.76 g, 20.2 mmol) were added thereto and stirred for 15 hours. After removal of methanol by distillation under reduced pressure, silica gel column-chromatography of the remaining residue was performed to give the title compound of white solid (1.2 g, 62%).

後処理

  1. stirringstirred for 15 hours
  2. customAfter removal of methanol
  3. distillationby distillation under reduced pressure, silica gel column-chromatography of the remaining residue

出典と根拠

ORDレコード
ord-3cd90ad7aae74a18947ca02117a2e167
出典データセット
uspto-grants-2013_03
特許番号
US08404696B2

反応ノート

読み込み中…