Hydrochloric Acid → HCID 44229381, 화합물

HRID 1951306노트

반응식

HRID 1951306 반응식
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

참가 물질

8

반응물 5

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

생성물 1

HCID 44229381HCID 44229381, 화합물

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-3cd90ad7aae74a18947ca02117a2e167
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404696B2

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