Dicyclohexylcarbodiimide → 2-Furancarboxylic acid, 5-methoxy-, 6-(aminoiminomethyl)-2-naphthalenyl ester, monomethanesulfonate

HRID 980020ノート

反応式

HRID 980020 の反応式
[CH3:1][O:2][C:3]1[O:7][C:6]([C:8]([OH:10])=[O:9])=[CH:5][CH:4]=1.C1CCC(N=C=NC2CCCCC2)CC1.[CH3:26][S:27]([O:30][C:31]1[CH:40]=[CH:39][C:38]2[C:33](=[CH:34][CH:35]=[C:36]([C:41](=[NH:43])[NH2:42])[CH:37]=2)[CH:32]=1)(=[O:29])=[O:28]>N1C=CC=CC=1>[CH3:26][S:27]([OH:30])(=[O:29])=[O:28].[CH3:1][O:2][C:3]1[O:7][C:6]([C:8]([O:10][C:31]2[CH:40]=[CH:39][C:38]3[C:33](=[CH:34][CH:35]=[C:36]([C:41](=[NH:42])[NH2:43])[CH:37]=3)[CH:32]=2)=[O:9])=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 7711072-Furancarboxylicacid,5-methoxy-(9CI)HCID 130505606-Carbamimidoylnaphthalen-2-yl methanesulfonate

生成物 1

HCID 211497772-Furancarboxylic acid, 5-methoxy-, 6-(aminoiminomethyl)-2-naphthalenyl ester, monomethanesulfonate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

In 10 ml of dry pyridine was dissolved 1.4 g of 5-methoxy-furan-2-carboxylic acid. To the resulting solution was added 2.5 g of DCC and the reaction mixture was stirred for 30 minutes at room temperature. To the reaction mixture was added with stirring and cooling in ice 2.8 g of 6-amidino-2-naphthol methanesulfonate. The reaction mixture was stirred overnight at room temperature. The precipitate was collected by filtration, washed with dry pyridine, added to DMF and stirred. The insolubles were filtered off and ethyl ether was added to the filtrate. The precipitate was collected by filtration and washed with acetone to obtain 2.7 g of 6-amidino-2-naphthyl 5-methoxy-furan-2-carboxylate methanesulfonate.

後処理

  1. additionTo the reaction mixture was added
  2. stirringwith stirring
  3. stirringThe reaction mixture was stirred overnight at room temperature
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with dry pyridine
  6. additionadded to DMF
  7. stirringstirred
  8. filtrationThe insolubles were filtered off
  9. additionethyl ether was added to the filtrate
  10. filtrationThe precipitate was collected by filtration
  11. washwashed with acetone

出典と根拠

ORDレコード
ord-6834421ff5a34401a947cc65f80287a3
出典データセット
uspto-grants-1987_01
特許番号
US04634783

反応ノート

読み込み中…