Sodium sulfide nonahydrate → 2-(2,3-Diamino-5-nitrophenyl)ethanol

HRID 477605

反応式

HRID 477605 の反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][C:5]([N+:11]([O-:13])=[O:12])=[CH:4][C:3]=1[CH2:14][CH2:15][OH:16].O.O.O.O.O.O.O.O.O.[S-2].[Na+].[Na+].[S]>C(O)(C)C.O>[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([N+:11]([O-:13])=[O:12])=[CH:4][C:3]=1[CH2:14][CH2:15][OH:16]

参加物

6

反応物 3

HCID 73972Sodium sulfide nonahydrateHCID 5362487SulfurHCID 198363402-(2-Amino-3,5-dinitrophenyl)ethanol

生成物 1

HCID 198363412-(2,3-Diamino-5-nitrophenyl)ethanol

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 3776Isopropanol溶媒

実験手順

To a suspension of 0.119 mole (27 g) of 2-(2-amino-3,5-dinitrophenyl)ethanol obtained in Example 1 in 67.5 ml of isopropanol to which an equal volume of water has been added, a solutionof 38.4 g of sodium sulphide nonahydrate and 5.4 g of sulphur in 10 ml of water is added dropwise at 60°-65° C. Heating is maintained for 20 minutes after the addition is complete. When the mixture is cooled, a precipitate of the expected product is obtained, and this is drained, made into a paste in water and then recrystallized from 96° strength alcohol. It melts at 172° C.

後処理

  1. additionhas been added
  2. temperatureHeating
  3. temperatureis maintained for 20 minutes
  4. additionafter the addition
  5. temperatureWhen the mixture is cooled

出典と根拠

ORDレコード
ord-cca36b5af0934f34967a86bcf8a390d3
出典データセット
uspto-grants-1989_12
特許番号
US04888445

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