Diisopropylethylamine → HCID 23043521、化合物

HRID 2165043ノート

反応式

HRID 2165043 の反応式
[NH2:1][CH2:2][CH2:3][NH:4][C:5](=[O:13])[CH2:6][N:7]1[CH2:11][CH2:10][CH2:9][C:8]1=[O:12].Br[CH2:15][CH2:16][Si:17]([CH2:20][CH2:21]Br)([CH3:19])[CH3:18].CCN(C(C)C)C(C)C>C(Cl)(Cl)Cl>[CH3:18][Si:17]1([CH3:19])[CH2:20][CH2:21][N:1]([CH2:2][CH2:3][NH:4][C:5](=[O:13])[CH2:6][N:7]2[CH2:11][CH2:10][CH2:9][C:8]2=[O:12])[CH2:15][CH2:16]1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 12169348Bis(2-bromoethyl)(dimethyl)silaneHCID 19908624HCID 19908624、化合物

生成物 1

HCID 23043521HCID 23043521、化合物収率 15%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A mixture of 1.90 g (10.3 mmol) of N-(2-aminoethyl)-2-oxo-1-pyrrolidineacetamide, 2.76 g (10.1 mmol) of bis(2-bromoethyl)dimethylsilane, 5.20 g of Huenig base, and 20 ml of chloroform was stirred and then the solvent was removed in vacuo. The resulting mixture was heated at 100°-105° C. for 8 hours. Aqueous NaHCO3 was added to the cooled reaction mixture, and the aqueous solution was extracted with chloroform. The dried chloroform solution was concentrated in vacuo and chromatographed on silica gel column to afford 450 mg (Yield: 15.0%) of the desired compound.

後処理

  1. customthe solvent was removed in vacuo
  2. temperatureThe resulting mixture was heated at 100°-105° C. for 8 hours
  3. additionAqueous NaHCO3 was added to the cooled reaction mixture
  4. extractionthe aqueous solution was extracted with chloroform
  5. concentrationThe dried chloroform solution was concentrated in vacuo
  6. customchromatographed on silica gel column

出典と根拠

ORDレコード
ord-2e8b07e7f01d404396ceb0de31adc2bc
出典データセット
uspto-grants-1990_07
特許番号
US04939126

反応ノート

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