Hydrochloric Acid → HCID 23158224, 화합물

HRID 601663노트

반응식

HRID 601663 반응식
C([Al]([CH2:6][CH3:7])CC)C.CNCCNC.C[O:15][C:16](=O)[C:17]1[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[N:19][C:18]=1[O:25][CH3:26].Cl>C1(C)C=CC=CC=1.CCCCCC>[CH3:26][O:25][C:18]1[C:17]([C:16](=[O:15])[CH2:6][CH3:7])=[CH:22][CH:21]=[C:20]([O:23][CH3:24])[N:19]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8070N,N'-DimethylethylenediamineHCID 10703069Methyl 2,6-dimethoxynicotinateHCID 16682930Triethylaluminum

생성물 1

HCID 23158224HCID 23158224, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매2회HCID 8058Hexane용매

실험 절차

Under nitrogen atmosphere, 15% hexane solution of triethyl aluminium was dropped at 0° C. to 26 m solution of toluene with 0.6 ml of N,N′-dimethyl-ethan-1,2-diamine, and the mixture was stirred at room temperature for 1 hour. Then, 5 ml solution of toluene with 1 g of 2,6-dimethoxy-nicotinic acid methylester was dropped at room temperature, and the mixture was stirred at 130° C. for 1 hour. The reaction solution was cooled down under ice temperature, 1M of hydrochloric acid was added, and extracted with ethyl acetate. Ethyl acetate layer was washed with saturated saline solution, dried with anhydrous sodium sulfate. The solvents were distilled outunder reduced pressure to obtain 156 mg of the above compound.

후처리

  1. stirringthe mixture was stirred at 130° C. for 1 hour
  2. additionwas added
  3. extractionextracted with ethyl acetate
  4. washEthyl acetate layer was washed with saturated saline solution
  5. dry with materialdried with anhydrous sodium sulfate
  6. distillationThe solvents were distilled outunder reduced pressure

출처 및 근거

ORD 기록
ord-ada68284eabd4dc8a978ddba728bc826
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902369B2

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