Water → 2-((2-Aminophenyl)amino)ethan-1-ol

HRID 1886050

反応式

HRID 1886050 の反応式
[N+:1]([C:4]1[CH:13]=[CH:12][CH:11]=[CH:10][C:5]=1[NH:6][CH2:7][CH2:8][OH:9])([O-])=O.Cl[Sn]Cl.O.[OH-].[Na+]>CCO>[NH2:1][C:4]1[CH:13]=[CH:12][CH:11]=[CH:10][C:5]=1[NH:6][CH2:7][CH2:8][OH:9]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 24479Stannous ChlorideHCID 78637HC Yellow No. 2

生成物 1

HCID 21140322-((2-Aminophenyl)amino)ethan-1-ol収率 86%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

According to the procedure of B. Agai, et al., Tetrahedron, 32, 839, (1976), a mixture of 2-(2-nitroanilino)ethanol (43.1 g, 0.237 mol), SnCl2.2 H2O (267.0 g, 1.18 mol), and EtOH (400 mL), was heated under reflux for 4 hours. The mixture was cooled, made basic (pH8) with 2.5N NaOH, and filtered through Celite. The filtrate was concentrated to remove the EtOH and the aqueous phase was extracted with EtOAc. The combined extracts were washed with H2O and brine, dried, and concentrated. Recrystallization from EtOH gave 31.0 g (86%) of a brown solid m.p. 105°-106° C.

後処理

  1. temperatureunder reflux for 4 hours
  2. temperatureThe mixture was cooled
  3. filtrationfiltered through Celite
  4. concentrationThe filtrate was concentrated
  5. customto remove the EtOH
  6. extractionthe aqueous phase was extracted with EtOAc
  7. washThe combined extracts were washed with H2O and brine
  8. customdried
  9. concentrationconcentrated
  10. customRecrystallization from EtOH

出典と根拠

ORDレコード
ord-08bb1e59f38047dc92ca8cb59ef45519
出典データセット
uspto-grants-1992_09
特許番号
US05149700

関連ノート

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