Diisopropylethylamine → HCID 68676237、化合物

HRID 2265811ノート

反応式

HRID 2265811 の反応式
F[B-](F)(F)F.[CH3:6][O+](C)C.[C:10]([N:13]1[C:21]2[C:16](=[CH:17][CH:18]=[C:19]([Cl:22])[CH:20]=2)[C:15](=[C:23]([OH:31])[C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([I:30])[CH:25]=2)[C:14]1=[O:32])(=[O:12])[CH3:11].C(N(C(C)C)C(C)C)C>ClCCl>[C:10]([N:13]1[C:21]2[C:16](=[CH:17][CH:18]=[C:19]([Cl:22])[CH:20]=2)[C:15](=[C:23]([O:31][CH3:6])[C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([I:30])[CH:25]=2)[C:14]1=[O:32])(=[O:12])[CH3:11]

参加物

5

反応物 3

HCID 81531Diisopropylethylamine2 回HCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)2 回HCID 178473965HCID 178473965、化合物2 回

生成物 1

HCID 68676237HCID 68676237、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A little at a time, 2.36 g of trimethyloxonium tetrafluoroborate are added to a solution of 3.52 g of 1-acetyl-3-[1-hydroxy-1-(3-iodophenyl)methylene]-6-chloro-2-indolinone (starting material VI) and 2.72 ml of ethyldiisopropylamine in 80 ml of dichloromethane, and the mixture is stirred at room temperature for one hour. Another 1.4 ml of ethyldiisopropylamine and 1.2 g of trimethyloxonium tetrafluoroborate are added, and the mixture is stirred at room temperature for another two hours. The mixture is then extracted with water and the organic phase is dried over magnesium sulphate and evaporated to dryness. The residue is recrystallized from ether and dried at 80° C. under reduced pressure.

後処理

  1. stirringthe mixture is stirred at room temperature for another two hours
  2. extractionThe mixture is then extracted with water
  3. dry with materialthe organic phase is dried over magnesium sulphate
  4. customevaporated to dryness
  5. customThe residue is recrystallized from ether
  6. customdried at 80° C. under reduced pressure

出典と根拠

ORDレコード
ord-c3173c2e2e074ce3874db2a301708fdc
出典データセット
uspto-grants-2010_12
特許番号
US07858616B2

反応ノート

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