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Ethylenediamine → HCID 22485685、化合物

HRID 2181191
ノート
印刷プレビュー

反応式

HRID 2181191 の反応式
[CH2:1]([O:4][CH:5]([CH2:9][C:10]1[CH:11]=[C:12]2[C:16](=[CH:17][CH:18]=1)[N:15](COCC[Si](C)(C)C)[CH:14]=[CH:13]2)[C:6]([OH:8])=[O:7])[CH2:2][CH3:3].C(N)CN.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>CN(C)C=O>[NH:15]1[C:16]2[C:12](=[CH:11][C:10]([CH2:9][CH:5]([O:4][CH2:1][CH2:2][CH3:3])[C:6]([OH:8])=[O:7])=[CH:18][CH:17]=2)[CH:13]=[CH:14]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 3301EthylenediamineHCID 2724141Tetrabutylammonium FluorideHCID 22485675HCID 22485675、化合物

生成物 1

HCID 22485685HCID 22485685、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

0.96 g rac-2-propoxy-3-[1-(2-trimethylsilanyl-ethoxymethyl)-1H-indol-5-yl]-propionic acid were dissolved in 40 ml N,N-dimethylformamide. 0.94 ml Ethylene diamine were added, followed by 7.63 ml of a tetra-butylammonium fluoride solution (1 molar in tetrahydrofuran); a small amount of molecular sieves was then added to the reaction mixture and it was heated to 80° C. After 6 hours, the mixture was cooled to r.t., filtered and the filtrate was poured into ice water and extracted 3 times with dichloromethane. The organic phases were washed with water, dried over MgSO4, filtered again and evaporated. The crude rac-3-(1H-indol-5-yl)-2-propoxy-propionic acid was used for the next step without purification.

後処理

  1. additiona small amount of molecular sieves was then added to the reaction mixture and it
  2. temperaturethe mixture was cooled to r.t.
  3. filtrationfiltered
  4. additionthe filtrate was poured into ice water
  5. extractionextracted 3 times with dichloromethane
  6. washThe organic phases were washed with water
  7. dry with materialdried over MgSO4
  8. filtrationfiltered again
  9. customevaporated
  10. customThe crude rac-3-(1H-indol-5-yl)-2-propoxy-propionic acid was used for the next step without purification

出典と根拠

ORDレコード
ord-20fef44b9b2e4258a7eab97bd2444a5c
出典データセット
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06890947B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート