Cesium carbonate → 2,6-dihydro-2-methyl-4-(2-methylpropyl)-6-[3,4,5-trimethoxyphenyl]methyl-1H-pyrrolo[3,4-d]pyridazin-1-one

HRID 1835149노트

반응식

HRID 1835149 반응식
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2=[CH:9][NH:10][CH:11]=[C:5]2[C:4]([CH2:12][CH:13]([CH3:15])[CH3:14])=[N:3]1.[CH3:16][O:17][C:18]1[CH:19]=[C:20]([CH:23]=[C:24]([O:28][CH3:29])[C:25]=1[O:26][CH3:27])[CH2:21]Cl.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C)C=O.Cl>[CH3:1][N:2]1[C:7](=[O:8])[C:6]2=[CH:9][N:10]([CH2:21][C:20]3[CH:23]=[C:24]([O:28][CH3:29])[C:25]([O:26][CH3:27])=[C:18]([O:17][CH3:16])[CH:19]=3)[CH:11]=[C:5]2[C:4]([CH2:12][CH:13]([CH3:15])[CH3:14])=[N:3]1

참가 물질

6

반응물 3

HCID 10796Cesium carbonateHCID 774485-(Chloromethyl)-1,2,3-trimethoxybenzeneHCID 1355247842-methyl-4-(2-methylpropyl)-1H,2H,6H-pyrrolo[3,4-d]pyridazin-1-one

생성물 1

HCID 235032722,6-dihydro-2-methyl-4-(2-methylpropyl)-6-[3,4,5-trimethoxyphenyl]methyl-1H-pyrrolo[3,4-d]pyridazin-1-one

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2,6-dihydro-2-methyl-4(2-methylpropyl)-1H-pyrrolo[3,4-d]pyridazin-1-one (Example 18 step a, 0.031 g), 3,4,5-trimethoxybenzyl chloride (0.038 g), and cesium carbonate (0.090 g) in dry dimethyl formamide (0.8 ml) was stirred for 16 hours, and then diluted with dilute hydrochloric acid. The mixture was extracted with ethyl acetate, which was washed with brine, dried, and evaporated to a solid. The solid was purified by chromatography on silica (dichloromethane/ethanol 9:1) to give 2,6-dihydro-2-methyl-4-(2-methylpropyl)-6-[3,4,5-trimethoxyphenyl]methyl-1H-pyrrolo[3,4-d]pyridazin-1-one (0.033 g).

후처리

  1. extractionThe mixture was extracted with ethyl acetate, which
  2. washwas washed with brine
  3. customdried
  4. customevaporated to a solid
  5. customThe solid was purified by chromatography on silica (dichloromethane/ethanol 9:1)

출처 및 근거

ORD 기록
ord-b61d3c651350422fbcff31dd2e27ea09
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06770646B2

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