Triethylamine → 1-(3-Phenyl-2-propenoyl)-1H-benzotriazo&

HRID 533493노트

반응식

HRID 533493 반응식
[C:1]([OH:11])(=O)/[CH:2]=[CH:3]/[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.CS([N:16]1[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[N:18]=[N:17]1)(=O)=O.C(N(CC)CC)C>O1CCCC1.C(#N)C>[N:16]1([C:1](=[O:11])/[CH:2]=[CH:3]/[C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[N:18]=[N:17]1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 444539Cinnamic Acid2회HCID 7920441-(Methylsulfonyl)-1H-benzotriazole

생성물 1

HCID 53382481-(3-Phenyl-2-propenoyl)-1H-benzotriazo&

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매

실험 절차

1.42 g (0.01 mol) of trans-cinnamic acid (compound of formula IV) and 1.97 g (0.01 mol) of 1-(methylsulfonyl)benzotriazole are stirred at room temperature in 50 ml of tetrahydrofuran, followed by dropwise addition of 0.014 mol of triethylamine. The solution is then refluxed for 24 hours, and then evaporated under reduced pressure. The residue is taken up in 60 ml of water and extracted with 70 ml of ethyl acetate. The organic phase is dried, filtered and then concentrated under vacuum. The powder obtained is taken up in 50 ml of acetonitrile and filtered off by suction.

후처리

  1. temperatureThe solution is then refluxed for 24 hours
  2. customevaporated under reduced pressure
  3. extractionextracted with 70 ml of ethyl acetate
  4. customThe organic phase is dried
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. customThe powder obtained
  8. filtrationfiltered off by suction

출처 및 근거

ORD 기록
ord-a3d2da41a7754e659006f4947e935aaf
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853276B2

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