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

HRID 477605

반응식

HRID 477605 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매2회HCID 3776Isopropanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-cca36b5af0934f34967a86bcf8a390d3
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04888445

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