Hydrochloric Acid → HCID 23158224、化合物

HRID 601663ノート

反応式

HRID 601663 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 23158224HCID 23158224、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒2 回HCID 8058Hexane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ada68284eabd4dc8a978ddba728bc826
出典データセット
uspto-grants-2011_03
特許番号
US07902369B2

反応ノート

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