Hydroxyamine hydrochloride → 2-(2-Ethyl-[1,3]dioxolan-2-yl)-2-fluoro-N-hydroxyacetamide

HRID 1096808ノート

反応式

HRID 1096808 の反応式
C[O:2][C:3](=O)[CH:4]([F:12])[C:5]1([CH2:10][CH3:11])[O:9][CH2:8][CH2:7][O:6]1.Cl.[NH2:15][OH:16].CO[Na]>N1C=CC=CC=1>[CH2:10]([C:5]1([CH:4]([F:12])[C:3]([NH:15][OH:16])=[O:2])[O:9][CH2:8][CH2:7][O:6]1)[CH3:11]

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 866370542-(2-Ethyl-[1,3]dioxolan-2-yl)fluoroacetic acid methyl esterHCID 178418582HCID 178418582、化合物

生成物 1

HCID 866370552-(2-Ethyl-[1,3]dioxolan-2-yl)-2-fluoro-N-hydroxyacetamide収率 40%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

実験手順

A mixture of 2-(2-ethyl-[1,3]dioxolan-2-yl)fluoroacetic acid methyl ester (1.50 g, 7.80 mmol) and hydroxylamine hydrochloride (1.07 g, 15.6 mmol) were dissolved in pyridine (8 mL). MeONa (30% in MeOH, 3.94 mL, 15.6 mmol) was dropped slowly over 15 min. More pyridine (8 mL) was added. The mixture was stirred for 30 min, then filtered. AcOH (1 mL) was added to the filtrate. The mixture was stirred for 5 min, then the solvents were removed under reduced pressure. Purification by FC (MeOH/CH2Cl2 1:10) yielded the title compound (502 mg, 40%).

後処理

  1. filtrationfiltered
  2. additionAcOH (1 mL) was added to the filtrate
  3. stirringThe mixture was stirred for 5 min
  4. customthe solvents were removed under reduced pressure
  5. customPurification by FC (MeOH/CH2Cl2 1:10)

出典と根拠

ORDレコード
ord-9c96e272269d434490d0cc1ca0de0521
出典データセット
uspto-grants-2012_03
特許番号
US08138340B2

反応ノート

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