HCID 57445398、化合物 → 4-(6-Benzyl-pyridazin-3-yl)-2-fluoro-phenol

HRID 1993365ノート

反応式

HRID 1993365 の反応式
[CH2:1]([C:8]1[N:9]=[N:10][C:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20]C)=[C:16]([F:22])[CH:15]=2)=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>B(Br)(Br)Br.C(Cl)Cl>[CH2:1]([C:8]1[N:9]=[N:10][C:11]([C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[C:16]([F:22])[CH:15]=2)=[CH:12][CH:13]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

3

反応物 1

HCID 57445398HCID 57445398、化合物

生成物 1

HCID 1360707044-(6-Benzyl-pyridazin-3-yl)-2-fluoro-phenol

試薬・触媒・溶媒 1

HCID 22277759Boron tribromide dichloromethane溶媒

実験手順

A solution of 3-benzyl-6-(3-fluoro-4-methoxy-phenyl)-pyridazine (Step 2, 1.5 g, 5.1 mmol) in 25 mL of 1 M BBr3/CH2Cl2 was stirred at RT for 16 h. The solution was then concentrated in vacuo and the residue was re-dissolved in 100 mL of EtOAc. The organic phase was washed with 40 mL of water followed by 40 mL of brine, dried over Na2SO4 and concentrated in vacuo to give the title compound. The solid has poor solubility in EtOAc and CH2Cl2 and was washed with 50% EtOAc/hexane and then used in the next step (yellow solid). MS (ESI pos. ion) m/z: 281.3 (M+H). Calc'd Exact Mass for C17H13FN2O: 280.30.

後処理

  1. concentrationThe solution was then concentrated in vacuo
  2. dissolutionthe residue was re-dissolved in 100 mL of EtOAc
  3. washThe organic phase was washed with 40 mL of water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f6694c79ff8a41e8b7738bd2e6628c63
出典データセット
uspto-grants-2010_01
特許番号
US07652009B2

反応ノート

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