Sodium Hydroxide → 2-Chloro-4-nitrobenzene-1-thiol

HRID 856700노트

반응식

HRID 856700 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1Br.[S:12]([O-])([O-])(=O)=O.[Na+].[Na+].[S].[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[SH:12]

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 24436Sodium SulfateHCID 346671-Bromo-2-chloro-4-nitrobenzeneHCID 5362487Sulfur

생성물 1

HCID 3057302-Chloro-4-nitrobenzene-1-thiol수율 58.6%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

2-chloro-4-nitro-bromobenzene (20 g) was dissolved in ethanol (160 ml), and an aqueous solution of sodium sulfate nanohydrate (15.2 g) and sulfur (2.0 g) in ethanol (200 ml) was added dropwise to the solution for 20 minutes under heat reflux. An aqueous solution of sodium hydroxide (5.1 g, 20.3 ml) was added dropwise to the solution for 20 minutes, and then, the mixture was cooled to room temperature, and ice-water was added thereto. The precipitates were filtered, and the pH of the filtrate was adjusted to about pH 5 with 6N hydrochloric acid, and the precipitates were collected by filtration and washed with water to give 2-chloro-4-nitrobenzenethiol (9.4 g).

후처리

  1. temperatureunder heat
  2. temperaturereflux
  3. filtrationThe precipitates were filtered
  4. filtrationthe precipitates were collected by filtration
  5. washwashed with water

출처 및 근거

ORD 기록
ord-03ca1855bbdb4537a14c920ca16daba2
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262185B2

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