Triethylamine → HCID 67494092、化合物

HRID 1968930ノート

反応式

HRID 1968930 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:19])=[C:6]([NH:8][C:9](=[O:18])/[CH:10]=[CH:11]/[C:12]2[CH:17]=[CH:16][CH:15]=CN=2)[CH:7]=1.[CH2:20]([N:22](CC)CC)C.[CH3:27][C:28]1[CH:36]=[CH:35][C:31]([C:32](Cl)=[O:33])=[CH:30][CH:29]=1.C(=O)([O-])[O-].[K+].[K+]>ClCCl>[CH3:19][C:5]1[CH:4]=[CH:3][C:2]([NH:1][C:32](=[O:33])[C:31]2[CH:35]=[CH:36][C:28]([CH3:27])=[CH:29][CH:30]=2)=[CH:7][C:6]=1[NH:8][C:9](=[O:18])[CH:10]=[CH:11][C:12]1[CH:20]=[N:22][CH:15]=[CH:16][CH:17]=1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 134054-Methylbenzoyl ChlorideHCID 86664945HCID 86664945、化合物

生成物 1

HCID 67494092HCID 67494092、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of the product of step 3 (0.25 g) and triethylamine (0.2 ml) in dichloromethane (25 ml), a solution of 4-methylbenzoyl chloride (0.5 g) in dichloromethane (10 ml) was added dropwise slowly in an ice-bath with the temperature no more than 5° C. After addition, the reaction was carried out for to 30 min in an ice-bath, and then at room temperature overnight. The completion of reaction was indicated by TLC. After that potassium carbonate solution (10%) was added, and then a solid was precipitated, and filtered out. The filter cake was washed with water, and recrystallized from ethyl acetate to give a solid.

後処理

  1. additionAfter addition
  2. customthe reaction was carried out for to 30 min in an ice-bath
  3. customat room temperature
  4. customovernight
  5. customThe completion of reaction
  6. customa solid was precipitated
  7. filtrationfiltered out
  8. washThe filter cake was washed with water
  9. customrecrystallized from ethyl acetate
  10. customto give a solid

出典と根拠

ORDレコード
ord-eedb9b2f82144a73bfd75213a84c032e
出典データセット
uspto-grants-2013_04
特許番号
US08426446B2

反応ノート

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