HC Yellow no. 14 → 3-Amino4-(2-hydroxyethylamino)benzonitrile

HRID 412552ノート

反応式

HRID 412552 の反応式
[OH:1][CH2:2][CH2:3][NH:4][C:5]1[CH:12]=[CH:11][C:8]([C:9]#[N:10])=[CH:7][C:6]=1[N+:13]([O-])=O.O.O.[Sn](Cl)(Cl)(Cl)Cl>C(O)C>[NH2:13][C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][C:5]=1[NH:4][CH2:3][CH2:2][OH:1])[C:9]#[N:10]

参加物

4

反応物 2

HCID 15001944HC Yellow no. 14HCID 85782573Tin tetrachloride dihydrate

生成物 1

HCID 185364343-Amino4-(2-hydroxyethylamino)benzonitrile収率 78.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 4-(2-hydroxyethylamino)-3-nitrobenzonitrile (3.11 g) and tin chloride dihydrate (16.94 g) in ethanol (50 ml) was stirred at 70° C. for 1 hour. After completion of the reaction, the solvent was evaporated and to the obtained residue were added tetrahydrofuran and 15% aqueous sodium hydroxide solution. The mixture was stirred and insoluble material and the aqueous layer were removed. The obtained organic layer was dried over anhydrous magnesium sulfate and the solvent was evaporated. The obtained solid was washed with chloroform, filtrated and dried under reduced pressure to give the title compound (2.08 g).

後処理

  1. customAfter completion of the reaction
  2. customthe solvent was evaporated and to the obtained residue
  3. additionwere added tetrahydrofuran and 15% aqueous sodium hydroxide solution
  4. custominsoluble material and the aqueous layer were removed
  5. dry with materialThe obtained organic layer was dried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated
  7. washThe obtained solid was washed with chloroform
  8. filtrationfiltrated
  9. customdried under reduced pressure

出典と根拠

ORDレコード
ord-7f4681a59657438b9c55441c2feb7f80
出典データセット
uspto-grants-2003_05
特許番号
US06562828B1

反応ノート

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