Acetic Acid → HCID 70031142、化合物

HRID 397534ノート

反応式

HRID 397534 の反応式
[NH2:1][C:2]1[C:3]([F:14])=[C:4]([CH2:9][C:10]([O:12][CH3:13])=[O:11])[C:5]([F:8])=[CH:6][CH:7]=1.CC(O)=O.[CH:19]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=1)=[CH2:20]>CO>[N:22]1[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=1[CH2:19][CH2:20][NH:1][C:2]1[C:3]([F:14])=[C:4]([CH2:9][C:10]([O:12][CH3:13])=[O:11])[C:5]([F:8])=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 75212-VinylpyridineHCID 10965547Methyl 2-(3-amino-2,6-difluorophenyl)acetate

生成物 1

HCID 70031142HCID 70031142、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 402 mg (2.0 mmol) of methyl 3-amino-2,6-difluorophenylacetate (prepared in step 3 of example 24) in 15 mL of MeOH was treated with 1.1 mL (20.0 mmol) of HOAc and 0.28 mL (2.6 mmol) of 2-vinylpyridine. The reaction mixture was stirred at reflux for 16 h. The mixture was cooled and the acetic acid was removed in vacuo. The residue was dissolved in EtOAc and washed with saturated NaHCO3 (4×5 mL), water (1×10 mL) and brine. Column chromatography (1:4 EtOAc/Hex) afforded methyl 3-(2-pyridylethyl)amino-2,6-difluorophenylacetate.

後処理

  1. temperatureat reflux for 16 h
  2. temperatureThe mixture was cooled
  3. customthe acetic acid was removed in vacuo
  4. dissolutionThe residue was dissolved in EtOAc
  5. washwashed with saturated NaHCO3 (4×5 mL), water (1×10 mL) and brine

出典と根拠

ORDレコード
ord-d57aae8940ad42a39594f288979475f2
出典データセット
uspto-grants-2003_08
特許番号
US06610701B2

反応ノート

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