Phosphorus tribromide → 5-Benzyloxy-2-[2-(4-bromomethyl-phenyl)-ethyl]-2H-pyridazin-3-one

HRID 564166ノート

反応式

HRID 564166 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[N:13][N:12]([CH2:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([CH2:23]O)=[CH:19][CH:18]=2)[C:11](=[O:25])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Br)(Br)[Br:27].C([O-])(O)=O.[Na+]>C(Cl)Cl>[CH2:1]([O:8][C:9]1[CH:14]=[N:13][N:12]([CH2:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([CH2:23][Br:27])=[CH:19][CH:18]=2)[C:11](=[O:25])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 24614Phosphorus tribromideHCID 516892Sodium BicarbonateHCID 670075955-Benzyloxy-2-[2-(4-hydroxymethyl-phenyl)-ethyl]-2H-pyridazin-3-one

生成物 1

HCID 670076305-Benzyloxy-2-[2-(4-bromomethyl-phenyl)-ethyl]-2H-pyridazin-3-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To 240 mg (0.71 mmol) 5-benzyloxy-2-[2-(4-hydroxymethyl-phenyl)-ethyl]-2H-pyridazin-3-one (example 21.1a) in 2.0 mL of DCM is added at 0° C. 134 μL (1.43 mmol) phosphorus tribromide. The mixture is stirred 4 h at RT, cooled to 0° C. and aqueous saturated NaHCO3-solution is added until pH >7. The layers are separated, the aqueous phase is extracted with DCM and the combined organic phase is washed with water, dried over MgSO4, filtered and the solvent is evaporated.

後処理

  1. temperaturecooled to 0° C.
  2. customThe layers are separated
  3. extractionthe aqueous phase is extracted with DCM
  4. washthe combined organic phase is washed with water
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-e17ffe1c877e47c2bd5825e80cb66eae
出典データセット
uspto-grants-2011_11
特許番号
US08067590B2

反応ノート

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