Triethylamine → HCID 67494092, 화합물

HRID 1968930노트

반응식

HRID 1968930 반응식
[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

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 134054-Methylbenzoyl ChlorideHCID 86664945HCID 86664945, 화합물

생성물 1

HCID 67494092HCID 67494092, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-eedb9b2f82144a73bfd75213a84c032e
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08426446B2

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