Tin atom → HCID 19035265, 화합물

HRID 263823노트

반응식

HRID 263823 반응식
[OH:1][CH2:2][CH2:3][NH:4][C:5]1[CH:10]=[C:9]([N+:11]([O-])=O)[C:8]([Cl:14])=[CH:7][C:6]=1[CH3:15].[Sn]>Cl.O.[OH-].[Na+]>[ClH:14].[NH2:11][C:9]1[C:8]([Cl:14])=[CH:7][C:6]([CH3:15])=[C:5]([NH:4][CH2:3][CH2:2][OH:1])[CH:10]=1

참가 물질

6

반응물 2

HCID 5352426Tin atomHCID 19035261HCID 19035261, 화합물

생성물 1

HCID 19035265HCID 19035265, 화합물

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 962Water용매HCID 14798Sodium Hydroxide용매

실험 절차

670 mg (2.9 mmol) of 2-(2'-hydroxyethyl)amino-5-chloro-4-nitrotoluene and 625 g of tin in 10 ml semiconcentrated hydrochloric acid were heated under reflux for one hour. After cooling, this mixture was diluted with 10 ml of water and 40 ml of 10 percent aqueous sodium hydroxide solution were added. The tin salt precipitate was filtered off and the filtrate was extracted 3 times with 30 ml of methylene chloride each time. After washing with water the filtrate was dried over sodium sulfate and the solvent was completely distilled away. The oily residue was received in 20 ml of methanol and reacted with an equimolar amount of hydrochloric acid.

후처리

  1. temperatureunder reflux for one hour
  2. temperatureAfter cooling
  3. additionwere added
  4. filtrationThe tin salt precipitate was filtered off
  5. extractionthe filtrate was extracted 3 times with 30 ml of methylene chloride each time
  6. washAfter washing with water the filtrate
  7. dry with materialwas dried over sodium sulfate
  8. distillationthe solvent was completely distilled away
  9. customreacted with an equimolar amount of hydrochloric acid

출처 및 근거

ORD 기록
ord-f8960cedc16c480fa010a7fa6ea85a33
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05645610

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