Hydrochloric Acid → 4-(4-Hydroxyphenylsulphanyl)-2-amino-nitrobenzene

HRID 1795865노트

반응식

HRID 1795865 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.[H-].[Na+].Cl[C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[C:14]([NH2:21])[CH:13]=1.Cl>CC(N(C)C)=O>[OH:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:12]2[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[C:14]([NH2:21])[CH:13]=2)=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 742185-Chloro-2-nitroanilineHCID 2401474-Mercaptophenol

생성물 1

HCID 221806834-(4-Hydroxyphenylsulphanyl)-2-amino-nitrobenzene수율 100.7%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

A solution of 4-hydroxybenzenethiol (46 g; 328 mmol) in DMA (500 ml) under argon was cooled to 0° C. and treated portionwise with NaH (28.9 g; 722 mmol; 60 % dispersion in oil). The mixture was stirred at room temperature for 2 hours and then solid 4-chloro-2-amino-nitrobenzene (56.6 g; 328 mmol) was added rapidly portionwise. The mixture was stirred and heated at 80° C. for 30 minutes and allowed to cool overnight. The mixture was poured into aqueous HCl (2 N) and the precipitate was filtered, washed with water, then pentane and dried in vacuo to give 4-(4-hydroxyphenylsulphanyl)-2-amino-nitrobenzene as a beige solid (86.6 g).

후처리

  1. stirringThe mixture was stirred
  2. temperatureheated at 80° C. for 30 minutes
  3. temperatureto cool overnight
  4. filtrationthe precipitate was filtered
  5. washwashed with water
  6. dry with materialpentane and dried in vacuo

출처 및 근거

ORD 기록
ord-fe814c29e71342e5955d3dc28f2d9fb2
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07030123B2

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