Dichloromethane → (2-Bromoethyl)tritylamine

HRID 373584

反応式

HRID 373584 の反応式
[C:1]1([C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)Cl)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.ClCCl.Br.[Br:25][CH2:26][CH2:27][NH2:28]>C(N(CC)CC)C>[Br:25][CH2:26][CH2:27][NH:28][C:7]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 6456Trityl chlorideHCID 27742172-Bromoethylamine hydrobromide

生成物 1

HCID 15718287(2-Bromoethyl)tritylamine

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

272.1 g (976 mmol) of triphenylchloromethane, 800 ml of dichloromethane and 200 g (976 mmol) of 2-bromoethanamine hydrobromide are introduced into a 2-1 round bottom flask placed under nitrogen. The mixture is stirred and 300 ml of triethylamine are added dropwise and stirring is continued for 48 h. The triethylamine hydrochloride which precipitates is separated off, water is added to the filtrate, the organic phase is separated off and is washed with water and dried over sodium sulphate, and the solvent is evaporated off. An oil is obtained, which is purified by chromatography on a column of silica gel. After recrystallisation from a mixture of dichloromethane and cyclohexane 273.17 g of white solid are obtained. Melting point: 108°-109° C.

後処理

  1. stirringstirring
  2. customThe triethylamine hydrochloride which precipitates
  3. customis separated off
  4. additionwater is added to the filtrate
  5. customthe organic phase is separated off
  6. washis washed with water
  7. dry with materialdried over sodium sulphate
  8. customthe solvent is evaporated off
  9. customAn oil is obtained
  10. customwhich is purified by chromatography on a column of silica gel
  11. customAfter recrystallisation
  12. additionfrom a mixture of dichloromethane and cyclohexane 273.17 g of white solid
  13. customare obtained

出典と根拠

ORDレコード
ord-276a018d26c74d3d84d0e19d06915cf1
出典データセット
uspto-grants-1992_11
特許番号
US05164397

関連ノート

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