Hydroxylamine → N'-hydroxy-1-oxo-1,3-dihydroisobenzofuran-5-carboximidamide

HRID 558002

反応式

HRID 558002 の反応式
[C:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:8](=[O:9])[O:7][CH2:6]2)#[N:2].[NH2:13][OH:14]>CCO>[OH:14][N:13]=[C:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:8](=[O:9])[O:7][CH2:6]2)[NH2:2]

参加物

4

反応物 2

HCID 787HydroxylamineHCID 8212181,3-Dihydro-1-oxoisobenzofuran-5-carbonitrile

生成物 1

HCID 59557669N'-hydroxy-1-oxo-1,3-dihydroisobenzofuran-5-carboximidamide収率 86.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 5-cyanophthalide (1 g, 6.28 mmol) and hydroxylamine (50% in water, 0.77 cm3, 0.83 g, 12.6 mmol, 2 eq) in EtOH (50 cm3) was stirred at room temperature for 60 hours and then under reflux for 3 hours. After cooling to room temperature and standing overnight, the solid formed was collected by filtration and dried in high vacuum line to give the product N′-hydroxy-1-oxo-1,3-dihydroisobenzofuran-5-carboximidamide (1.04 g, 86.2%) as a white solid, mp 223-226° C. (decomposed).

後処理

  1. temperatureunder reflux for 3 hours
  2. customthe solid formed
  3. filtrationwas collected by filtration
  4. customdried in high vacuum line

出典と根拠

ORDレコード
ord-60166204d24d4020b62ff07a5b7003bd
出典データセット
uspto-grants-2011_11
特許番号
US08062429B2

関連ノート

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