Sodium methanethiolate → HCID 68980262, 화합물

HRID 1783726노트

반응식

HRID 1783726 반응식
[CH3:1][S-:2].[Na+].[Br:4][C:5]1[C:14]2[C:9](=[CH:10][C:11]([CH2:15]Br)=[CH:12][CH:13]=2)[C:8](=[O:17])[N:7]([CH:18]([CH3:20])[CH3:19])[N:6]=1>C1COCC1>[Br:4][C:5]1[C:14]2[C:9](=[CH:10][C:11]([CH2:15][S:2][CH3:1])=[CH:12][CH:13]=2)[C:8](=[O:17])[N:7]([CH:18]([CH3:20])[CH3:19])[N:6]=1

참가 물질

4

반응물 2

HCID 4378561Sodium methanethiolateHCID 211065684-Bromo-7-bromomethyl-2-isopropyl-2H-phthalazin-1-one

생성물 1

HCID 68980262HCID 68980262, 화합물수율 79.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Sodium methanethiolate (0.23 g, 3.33 mmol) was dissolved in THF (1 ml) and added dropwise to a solution of 4-bromo-7-bromomethyl-2-isopropyl-2H-phthalazin-1-one (0.4 g, 1.11 mmol) in THF (10 ml). The mixture was stirred at RT for 3 hours whereupon LC-MS indicated complete consumption of starting material. The reaction mixture was diluted with water (20 ml) and extracted with EtOAc (50 ml). The organic layer was separated, dried (MgSO4), filtered and concentrated under vacuum. The residue was subjected to flash column chromatography (elution: 80% heptane, 20% EtOAc) to give the title compound (0.29 g, 79% yield) as a white solid.

후처리

  1. customconsumption of starting material
  2. additionThe reaction mixture was diluted with water (20 ml)
  3. extractionextracted with EtOAc (50 ml)
  4. customThe organic layer was separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum
  8. washThe residue was subjected to flash column chromatography (elution: 80% heptane, 20% EtOAc)

출처 및 근거

ORD 기록
ord-84790ff519744daea89f8d0679fadac8
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07501410B2

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