Diisopropylethylamine → HCID 68676237, 화합물

HRID 2265811노트

반응식

HRID 2265811 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-c3173c2e2e074ce3874db2a301708fdc
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858616B2

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