Water → HCID 69344008, 화합물

HRID 590538노트

반응식

HRID 590538 반응식
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])([O-])=O.[K+].[K+].Br[CH2:16][CH2:17][Si:18]([CH2:21][CH2:22]Br)([CH3:20])[CH3:19].O>ClCCl>[CH2:1]([N:8]1[CH2:22][CH2:21][Si:18]([CH3:20])([CH3:19])[CH2:17][CH2:16]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 7504BenzylamineHCID 11430Potassium CarbonateHCID 12169348Bis(2-bromoethyl)(dimethyl)silane

생성물 1

HCID 69344008HCID 69344008, 화합물수율 59%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Benzylamine (17.56 g, 0.16 mol) and K2CO3 (3.4 g, 24.6 mmol) are added to a solution of bis(2-bromoethyl)dimethylsilane 2(4.0 g, 16.4 mmol) in Dichloromethane (DCM). The mixture is then refluxed for 16 h. Water is added and the aqueous layer is extracted with DCM. It is then washed with 5% sodiumhydroxide (NaOH) solution, dried and concentrated. The product is purified by column chromatography on silica using hexane-ethylacetate mixtures to obtain the product as a colorless liquid 3 (2.1 g) in 59% yield.

후처리

  1. temperatureThe mixture is then refluxed for 16 h
  2. extractionthe aqueous layer is extracted with DCM
  3. washIt is then washed with 5% sodiumhydroxide (NaOH) solution
  4. customdried
  5. concentrationconcentrated
  6. customThe product is purified by column chromatography on silica

출처 및 근거

ORD 기록
ord-0062cea83da548a190c00b6c7564fcb6
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09233989B2

반응 노트

불러오는 중…