Diisopropylethylamine → HCID 68676237, 화합물

HRID 1376203노트

반응식

HRID 1376203 반응식
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]

참가 물질

5

반응물 3

HCID 81531Diisopropylethylamine2회HCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)2회HCID 178473965HCID 178473965, 화합물2회

생성물 1

HCID 68676237HCID 68676237, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-14f09d1a060741e8bac366ae8c4329c2
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07169936B2

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