Diisopropylethylamine → HCID 68676237、化合物

HRID 2109017ノート

反応式

HRID 2109017 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

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

2.36 g of trimethyloxonium tetrafluoroborate are added batchwise to a solution of 3.52 g of 1-acetyl-3-[1-hydroxy-1-(3-iodo-phenyl)-methylene]-6-chloro-2-indolinone (educt VII) and 2.72 ml of ethyldiisopropylamine in 80 ml dichloromethane and the mixture is stirred for one hour at ambient temperature. Then another 1.4 ml ethyldiisopropylamine and 1.2 g trimethyloxonium tetrafluoroborate are added and the mixture is stirred for a further two hours at ambient temperature. Then it is extracted with water, the organic phase is dried over magnesium sulphate and evaporated to dryness. The residue is recrystallised from ether and dried in vacuo at 80° C.

後処理

  1. stirringthe mixture is stirred for a further two hours at ambient temperature
  2. extractionThen it is extracted with water
  3. dry with materialthe organic phase is dried over magnesium sulphate
  4. customevaporated to dryness
  5. customThe residue is recrystallised from ether
  6. customdried in vacuo at 80° C.

出典と根拠

ORDレコード
ord-ec0b5c69946949bb867b5cc39ebb2471
出典データセット
uspto-grants-2009_04
特許番号
US07514468B2

反応ノート

読み込み中…