Methanesulfonic Acid → 2-Methyl-1-[1-methyl-2-[(2,6-dimethylphenyl)carbamoyl]ethyl]-2-imidazoline

HRID 223385노트

반응식

HRID 223385 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][C:10](=[O:14])/[CH:11]=[CH:12]/[CH3:13].[CH3:15][C:16]1[NH:20][CH2:19][CH2:18][N:17]=1.CS(O)(=O)=O>C(O)C>[CH3:15][C:16]1[N:20]([CH:12]([CH3:13])[CH2:11][C:10](=[O:14])[NH:9][C:3]2[C:2]([CH3:1])=[CH:7][CH:6]=[CH:5][C:4]=2[CH3:8])[CH2:19][CH2:18][N:17]=1

참가 물질

5

반응물 3

HCID 6395Methanesulfonic AcidHCID 107982-MethylimidazolineHCID 6061099N-(2,6-dimethylphenyl)crotonamide

생성물 1

HCID 204806282-Methyl-1-[1-methyl-2-[(2,6-dimethylphenyl)carbamoyl]ethyl]-2-imidazoline

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Combine 1.89 gm. (0.01 M) N-(2,6-dimethylphenyl)crotonamide, 0.90 gm. (0.0107 M) lysidine, 0.01 gm. (~0.001 M) methanesulphonic acid and about 40 ml. of ethanol in a pressure bottle and heat (bath temp. 100°-110° C.) for about 100 hours. Remove the solvent in vacuo, add about 50 ml. of water. Adjust the pH to 8.0 with concentrated HCl, and extract the aqueous phase with 2×25 ml. methylene chloride. Then adjust the aqueous phase to pH 13 with 50% sodium hydroxide and extract with 3×30 ml. of methylene chloride. Wash the combined methylene chloride extracts with 2×5 ml. of water. Dry the methylene chloride extracts over sodium sulfate. Evaporate off the solvents to obtain the title compound.

후처리

  1. customRemove the solvent in vacuo
  2. additionadd about 50 ml
  3. extractionextract the aqueous phase with 2×25 ml
  4. extractionextract with 3×30 ml
  5. washWash the combined methylene chloride
  6. dry with materialDry the methylene chloride
  7. customEvaporate off the solvents

출처 및 근거

ORD 기록
ord-96edf798c4604c18b309536b044217db
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04353921

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