Sodium Hydroxide → HCID 178490208, 화합물

HRID 26815

반응식

HRID 26815 반응식
NC(N)=[S:3].[CH3:5][O:6][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][C:14]=1[O:15][CH3:16])[CH2:10]Cl.[OH-].[Na+].Cl[CH2:20][C:21]([O-:23])=O.[Na+]>O>[CH3:5][O:6][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][C:14]=1[O:15][CH3:16])[CH2:10][CH2:20][C:21]([OH:23])=[S:3]

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 81740Veratryl chlorideHCID 2723790ThioureaHCID 23665759Sodium chloroacetate

생성물 1

HCID 178490208HCID 178490208, 화합물수율 69%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

13.07 g (0.172 mol) of thiourea and 86 ml of water are introduced into a 1 liter 3-necked flask equipped with a magnetic stirrer and a condenser. The mixture is heated to 50°-60° C. and 32 g (0.172 mol) of 3,4-dimethoxybenzylchloride are added in a single operation. The reactants are heated to reflux and boiling is maintained for 15 mins; the solution becomes limpid. Thereafter the mixture is cooled and a solution of 27.52 g (0.688 mol) of NaOH in 43 ml of water is introduced dropwise at about 60° C. Heating under reflux is again carried out for 30 minutes, the mixture is cooled and a solution of sodium chloroacetate (obtained by neutralising 22.76 g of chloroacetic acid in 172 ml of water with 20.23 g of NaHCO3) is added dropwise at 60°-70° C. The whole is then heated under reflux for 30 minutes, cooled, filtered and then acidified with 3 N HCl. After recrystallisation from toluene, 28.7 g of 3,4-dimethoxybenzylthio-acetic acid are obtained. Yield: 69%. Instantaneous melting point: 94° C.

후처리

  1. customequipped with a magnetic stirrer and a condenser
  2. temperatureThe mixture is heated to 50°-60° C.
  3. temperatureThe reactants are heated
  4. temperatureto reflux
  5. temperatureboiling is maintained for 15 mins
  6. temperatureThereafter the mixture is cooled
  7. temperatureHeating
  8. temperatureunder reflux
  9. temperaturethe mixture is cooled
  10. temperatureThe whole is then heated
  11. temperatureunder reflux for 30 minutes
  12. temperaturecooled
  13. filtrationfiltered
  14. customAfter recrystallisation from toluene, 28.7 g of 3,4-dimethoxybenzylthio-acetic acid
  15. customare obtained

출처 및 근거

ORD 기록
ord-a179228e5546415b814b3f7390e0f9f7
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151300

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