Hydrochloric Acid → HCID 13103759, 화합물

HRID 354685노트

반응식

HRID 354685 반응식
[CH3:1][O:2][C:3]1[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH3:24])=[CH:17][C:4]=1[CH2:5][CH:6]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:7]([O:9][CH2:10][CH3:11])=[O:8].[H-].[Na+].[Cl:27]N1C(=O)CCC1=O.Cl>O1CCCC1.O>[Cl:27][C:6]([CH2:5][C:4]1[CH:17]=[C:18]([O:23][CH3:24])[C:19]([O:21][CH3:22])=[CH:20][C:3]=1[O:2][CH3:1])([C:7]([O:9][CH2:10][CH3:11])=[O:8])[C:12]([O:14][CH2:15][CH3:16])=[O:13]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 31398ChlorosuccinimideHCID 13103753Diethyl 2,4,5-trimethoxybenzylmalonate

생성물 1

HCID 13103759HCID 13103759, 화합물수율 91.5%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

In 70 ml of anhydrous tetrahydrofuran is dissolved 6.5 g of diethyl 2,4,5-trimethoxybenzylmalonate and, then, 760 mg of 60% oily sodium hydride is added. The mixture is stirred at room temperature for 15 minutes, after which time 2.54 g of N-chlorosuccinimide is added. The mixture is further stirred at room temperature for 30 minutes. The reaction mixture is poured into a mixture of 300 ml water and 10 ml 6N-HCl and, then, extracted with ether. The ethereal layer is washed with water, dried (over MgSO4) and distilled to remove the ether, whereupon 6.5 g (91.5%) of diethyl α-chloro-α-(2,4,5-trimethoxybenzyl)malonate is obtained as crystals melting at 84°-85° C.

후처리

  1. stirringThe mixture is further stirred at room temperature for 30 minutes
  2. extractionextracted with ether
  3. washThe ethereal layer is washed with water
  4. dry with materialdried (over MgSO4)
  5. distillationdistilled
  6. customto remove the ether

출처 및 근거

ORD 기록
ord-906a4fdce16a4e0aaf9d3ce3b45d2b50
출처 데이터셋
uspto-grants-1983_03
특허 번호
US04376777

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