Sodium Cyanate → 3-(N-Carbamoyl-4-aminobutyl)-9,10-dimethoxy-2-(2,4,6-trimethylphenylimino)-3,4,6,7-tetrahydro-2H-pyrimido[6,1-a]isoquinolin-4-one

HRID 884513노트

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HRID 884513 반응식
[O-:1][C:2]#[N:3].[Na+].[NH2:5][CH2:6][CH2:7][CH2:8][CH2:9][N:10]1[C:27](=[N:28][C:29]2[C:34]([CH3:35])=[CH:33][C:32]([CH3:36])=[CH:31][C:30]=2[CH3:37])[CH:26]=[C:13]2[C:14]3[C:19]([CH2:20][CH2:21][N:12]2[C:11]1=[O:38])=[CH:18][C:17]([O:22][CH3:23])=[C:16]([O:24][CH3:25])[CH:15]=3>O.Cl>[C:2]([NH:5][CH2:6][CH2:7][CH2:8][CH2:9][N:10]1[C:27](=[N:28][C:29]2[C:34]([CH3:35])=[CH:33][C:32]([CH3:36])=[CH:31][C:30]=2[CH3:37])[CH:26]=[C:13]2[C:14]3[C:19]([CH2:20][CH2:21][N:12]2[C:11]1=[O:38])=[CH:18][C:17]([O:22][CH3:23])=[C:16]([O:24][CH3:25])[CH:15]=3)(=[O:1])[NH2:3]

참가 물질

5

반응물 2

HCID 517096Sodium CyanateHCID 219584963-(4-Aminobutyl)9,10-dimethoxy-2-(2,4,6-trimethylphenylimino)-3,4,6,7-tetrahydro-2H-pyrimido[6,1-a]isoquinolin-4-one

생성물 1

HCID 99359563-(N-Carbamoyl-4-aminobutyl)-9,10-dimethoxy-2-(2,4,6-trimethylphenylimino)-3,4,6,7-tetrahydro-2H-pyrimido[6,1-a]isoquinolin-4-one수율 64.1%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매2회

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온도
80 °C

실험 절차

Sodium cyanate (0.28 g, 4.32 mmol) in water (6 ml) was added dropwise to a stirred solution of 2 (1.0 g, 2.16 mmol) in water (30 ml) and 1N HCl (4.3 ml) at 80° C. After 2 h at 80° C. the mixture was cooled and extracted with dichloromethane (3×20 ml) and the extract dried (MgSO4) and evaporated in vacuo. The residue was purified by column chromatography on silica gel [dichloromethane/methanol (97:3)] to obtain the title compound (0.70 g, 64%) as a yellow solid.

후처리

  1. extractionextracted with dichloromethane (3×20 ml)
  2. dry with materialthe extract dried (MgSO4)
  3. customevaporated in vacuo
  4. customThe residue was purified by column chromatography on silica gel [dichloromethane/methanol (97:3)]

출처 및 근거

ORD 기록
ord-5c5e79ccb4a04567aa14519a10e7eb75
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08242127B2

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