Hydrochloric Acid → 2-Chloromethyl-5-dimethylaminomethyl-3-methylfuran

HRID 1702342

반응식

HRID 1702342 반응식
[CH3:1][N:2]([CH2:4][C:5]1[O:6][CH:7]=[CH:8][C:9]=1C)[CH3:3].[CH2:11]=O.Cl.[CH:14]([Cl:17])(Cl)Cl>[Cl-].[Zn+2].[Cl-]>[Cl:17][CH2:14][C:7]1[O:6][C:5]([CH2:4][N:2]([CH3:1])[CH3:3])=[CH:9][C:8]=1[CH3:11]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 712Formaldehyde2회HCID 6212ChloroformHCID 100347492-Dimethylaminomethyl-3-methylfuran

생성물 1

HCID 204020362-Chloromethyl-5-dimethylaminomethyl-3-methylfuran

시약·촉매·용매 1

HCID 3007855Zincchloride촉매

실험 절차

To a solution of 2-dimethylaminomethyl-3-methylfuran (6.5 g; 37.0 mmoles) [prepared in Step A] in 250 ml of chloroform was added paraformaldehyde (1.67 g; 55.7 mmoles) and zinc chloride (312 mg), and a slow stream of HCl gas was bubbled through while stirring at ambient temperature for 15 minutes. Stirring was continued for 2 hours, then HCl gas was bubbled through for 15 minutes and the mixture stirred for 1 hour. At this time additional paraformaldehyde (1.67 g; 55.7 mmoles) was added to the reaction mixture and a slow stream of HCl gas was passed through for 15 minutes. After stirring at ambient temperature for 18 hours, the reaction mixture was filtered through Celite and the filtrate evaporated under reduced pressure to yield the title compound (4.97 g) which crystallized upon standing and was used without further purification in Step C.

후처리

  1. customa slow stream of HCl gas was bubbled through
  2. stirringStirring
  3. waitwas continued for 2 hours
  4. customHCl gas was bubbled through for 15 minutes
  5. stirringthe mixture stirred for 1 hour
  6. customwas passed through for 15 minutes
  7. stirringAfter stirring at ambient temperature for 18 hours
  8. filtrationthe reaction mixture was filtered through Celite
  9. customthe filtrate evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-17c89b0b8bc240afb413485fcba6c4a5
출처 데이터셋
uspto-grants-1983_04
특허 번호
US04380639

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