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

HRID 533493ノート

反応式

HRID 533493 の反応式
[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

参加物

6

反応物 3

HCID 8471TriethylamineHCID 444539Cinnamic Acid2 回HCID 7920441-(Methylsulfonyl)-1H-benzotriazole

生成物 1

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

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a3d2da41a7754e659006f4947e935aaf
出典データセット
uspto-grants-2014_10
特許番号
US08853276B2

反応ノート

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