Hydrochloric Acid → 2-(4-Fluorobenzyl)-10-methoxy-4-(1-hydroxyethyl)-8-methyl-7,8-dihydropyrazino[1',2':1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione

HRID 494130노트

반응식

HRID 494130 반응식
[F:1][C:2]1[CH:28]=[CH:27][C:5]([CH2:6][N:7]2[C:12](=[O:13])[C:11]3[C:14]([O:23][CH3:24])=[C:15]4[C:20](=[O:21])[N:19]([CH3:22])[CH2:18][CH2:17][N:16]4[C:10]=3[C:9]([CH:25]=[O:26])=[N:8]2)=[CH:4][CH:3]=1.[CH3:29][Mg]Br.C(OCCCC)CCC.Cl>COCCOC.ClCCl>[F:1][C:2]1[CH:28]=[CH:27][C:5]([CH2:6][N:7]2[C:12](=[O:13])[C:11]3[C:14]([O:23][CH3:24])=[C:15]4[C:20](=[O:21])[N:19]([CH3:22])[CH2:18][CH2:17][N:16]4[C:10]=3[C:9]([CH:25]([OH:26])[CH3:29])=[N:8]2)=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8909Butyl etherHCID 866248002-(4-Fluorobenzyl)-8-methyl-10-methoxy-1,9-dioxo-1,2,6,7,8,9-hexahydropyrazino[1',2':1,5]pyrrolo[2,3-d]pyridazine-4-carboxaldehydeHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 688652402-(4-Fluorobenzyl)-10-methoxy-4-(1-hydroxyethyl)-8-methyl-7,8-dihydropyrazino[1',2':1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 80711,2-Dimethoxyethane용매

실험 절차

To a solution of 2-(4-fluorobenzyl)-8-methyl-10-methoxy-1,9-dioxo-1,2,6,7,8,9-hexahydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-4-carboxaldehyde (42 mg, 0.11 mmol) in anhydrous DME (10 mL), a solution of methyl magnesium bromide in butyl ether (0.26 mL, 0.26 mmol; 1 M) was added. After stirring at room temperature for 5 minutes, the reaction mixture was treated with dilute hydrochloric acid, and diluted with dichloromethane. The organic extract was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated under vacuum to provide the title compound as yellow solid. ES MS M+1=401

후처리

  1. extractionThe organic extract
  2. washwas washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-6b80db1d61604f87888245a5bbeadb0c
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538112B2

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