Diisopropylethylamine → HCID 68676237, 화합물

HRID 2109017노트

반응식

HRID 2109017 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, 화합물

생성물 1

HCID 68676237HCID 68676237, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-ec0b5c69946949bb867b5cc39ebb2471
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07514468B2

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