Water → HCID 69344008、化合物

HRID 590538ノート

反応式

HRID 590538 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 69344008HCID 69344008、化合物収率 59%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0062cea83da548a190c00b6c7564fcb6
出典データセット
uspto-grants-2016_01
特許番号
US09233989B2

反応ノート

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