Hydrochloric Acid → HCID 178490206, 화합물

HRID 2188726노트

반응식

HRID 2188726 반응식
[OH-:1].[Na+].[CH2:3]([SH:7])[C:4](O)=O.[CH3:8][O:9][C:10]1[CH:17]=[CH:16][C:13]([CH2:14]Cl)=[CH:12][C:11]=1[N+:18]([O-:20])=[O:19].Cl>CO>[CH3:8][O:9][C:10]1[CH:17]=[CH:16][C:13]([CH2:14][CH2:4][C:3]([OH:1])=[S:7])=[CH:12][C:11]=1[N+:18]([O-:20])=[O:19]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1133Thioglycolic AcidHCID 14798Sodium HydroxideHCID 807854-(Chloromethyl)-2-nitroanisole

생성물 1

HCID 178490206HCID 178490206, 화합물수율 95%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a cold solution of sodium hydroxide (9.75 g, 240 mmol) in methanol (200 mL), thioglycollic acid (11.25 g, 120 mmol) was added slowly over 30 minutes. Sodium thioglycollate precipitated was dissolved by stirring and warming up the solution. The solution was cooled to room temperature and 4-methoxy-3-nitrobenzyl chloride (30.0 g, 120 mmol) was added in portions to reduce the intensity of exothermic reaction. The reaction mixture was then refluxed for 4 hours, cooled and poured onto crushed ice (1 Kg) containing hydrochloric acid (50 mL). The precipitate formed was filtered, washed with ice cold water and dried under vacuum. (30.0 g, 95% yield) m.p. 130-132° C.

후처리

  1. customSodium thioglycollate precipitated
  2. dissolutionwas dissolved
  3. temperaturewarming up the solution
  4. customthe intensity of exothermic reaction
  5. temperatureThe reaction mixture was then refluxed for 4 hours
  6. temperaturecooled
  7. additionpoured
  8. customThe precipitate formed
  9. filtrationwas filtered
  10. washwashed with ice cold water
  11. customdried under vacuum

출처 및 근거

ORD 기록
ord-daef8d6352984c808ad7756fd6f77bf5
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08324190B2

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