Potassium Phosphate, Tribasic → 6-Bromoimidazo[1,2-a]pyridin-2-amine

HRID 555984ノート

反応式

HRID 555984 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([NH:11]C(=O)C(F)(F)F)[N:10]=2)[CH:7]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>COCCOC>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([NH2:11])[N:10]=2)[CH:7]=1

参加物

4

反応物 2

HCID 62657Potassium Phosphate, TribasicHCID 12065953N-{6-bromoimidazo[1,2-a]pyridin-2-yl}-2,2,2-trifluoroacetamide

生成物 1

HCID 441192966-Bromoimidazo[1,2-a]pyridin-2-amine

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

A stirred solution of N-(6-bromo-imidazo[1,2-a]pyridin-2-yl)-2,2,2-trifluoro-acetamide (9.0 g, 29.2 mmol) in DME (90 ml) and 1.27 M aqueous potassium phosphate (80.5 ml, 102.3 mmol) is heated at 90° C. overnight. After cooling to room temperature, the two layers are separate and the aqueous portion is extracted with EtOAc. The combined organic extracts are concentrated in vacuo to afford a brown oil. Iso-hexanes is added to the oil resulting in the formation of a solid. The excess iso-hexanes is decanted off and the remaining DME is azeotroped with THF (2×50 ml) to afford the title compound as a solid [MH+ 211.93].

後処理

  1. customthe two layers are separate
  2. extractionthe aqueous portion is extracted with EtOAc
  3. concentrationThe combined organic extracts are concentrated in vacuo
  4. customto afford a brown oil
  5. customresulting in the formation of a solid
  6. customThe excess iso-hexanes is decanted off
  7. customthe remaining DME is azeotroped with THF (2×50 ml)

出典と根拠

ORDレコード
ord-09f3c55c328649578162ddb714c4b524
出典データセット
uspto-grants-2011_11
特許番号
US08053574B2

反応ノート

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