Sodium methanethiolate → HCID 68980262、化合物

HRID 1783726ノート

反応式

HRID 1783726 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 68980262HCID 68980262、化合物収率 79.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-84790ff519744daea89f8d0679fadac8
出典データセット
uspto-grants-2009_03
特許番号
US07501410B2

反応ノート

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