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Dicyclohexylcarbodiimide → 6-Amidino-1-(2-carbamoylvinyl)-2-naphthyl 4-aminoiminomethylaminobenzoate.dihydrochloride

HRID 1419256
ノート
印刷プレビュー

反応式

HRID 1419256 の反応式
[NH2:1][N:2]=[CH:3][NH:4][C:5]1[CH:13]=[CH:12][C:8]([C:9]([OH:11])=[O:10])=[CH:7][CH:6]=1.CS([O-])(=O)=O.[ClH:19].[C:20]([C:23]1[CH:24]=[C:25]2[C:30](=[CH:31][CH:32]=1)[C:29]([CH:33]=[CH:34][C:35](=[O:37])[NH2:36])=[C:28](O)[CH:27]=[CH:26]2)(=[NH:22])[NH2:21].C1CCC(N=C=NC2CCCCC2)CC1>CN(C1C=CN=CC=1)C.N1C=CC=CC=1>[ClH:19].[ClH:19].[NH2:1][N:2]=[CH:3][NH:4][C:5]1[CH:13]=[CH:12][C:8]([C:9]([O:11][C:28]2[CH:27]=[CH:26][C:25]3[C:30](=[CH:31][CH:32]=[C:23]([C:20](=[NH:21])[NH2:22])[CH:24]=3)[C:29]=2[CH:33]=[CH:34][C:35](=[O:37])[NH2:36])=[O:10])=[CH:7][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 10868DicyclohexylcarbodiimideHCID 85257MethanesulfonateHCID 1372316906-Amidino-1-(2-carbamoylvinyl)-2-naphthol.hydrochlorideHCID 178514393HCID 178514393、化合物

生成物 1

HCID 1784787626-Amidino-1-(2-carbamoylvinyl)-2-naphthyl 4-aminoiminomethylaminobenzoate.dihydrochloride収率 180.2%

試薬・触媒・溶媒 2

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 1049Pyridine溶媒

実験手順

90 Milliliters of 20% hydrous pyridine was added to 5.08 g of 4-aminoiminomethylaminobenzoic acid.methanesulfonate, 4.5 g of 6-amidino-1-(2-carbamoylvinyl)-2-naphthol.hydrochloride, 6.34 g of DCC and 80 mg of DMAP, followed by stirring for 2 hours under cooling with ice and then 48 hours at room temperature. Then, the precipitate was collected by filtration and washed twice with 160 ml of warm 20% hydrous pyridine. The above-obtained reaction filtrate and the warm hydrous pyridine wash liquid were combined and the resulting solution was added to 1 liter of acetone, followed by stirring for 24 hours under cooling with ice. The precipitate was collected by filtration and thereto was added 70 ml of warm DMF to dissolve the precipitate. Then, 0.5 g of active carbon was added, followed by stirring for 30 minutes at room temperature. Insoluble matter was filtered and 8.4 ml of concentrated hydrochloric acid was added to the filtrate. The resulting solution was added dropwise to 600 ml of acetone, followed by stirring for 24 hours under cooling with ice. Then, the precipitate was collected by filtration to obtain 6.8 g of the desired product.

後処理

  1. temperatureunder cooling with ice
  2. custom48 hours
  3. customat room temperature
  4. filtrationThen, the precipitate was collected by filtration
  5. washwashed twice with 160 ml of warm 20% hydrous pyridine
  6. customThe above-obtained reaction filtrate
  7. washthe warm hydrous pyridine wash liquid
  8. additionthe resulting solution was added to 1 liter of acetone
  9. stirringby stirring for 24 hours
  10. temperatureunder cooling with ice
  11. filtrationThe precipitate was collected by filtration
  12. additionwas added 70 ml of warm DMF
  13. dissolutionto dissolve the precipitate
  14. additionThen, 0.5 g of active carbon was added
  15. stirringby stirring for 30 minutes at room temperature
  16. filtrationInsoluble matter was filtered
  17. addition8.4 ml of concentrated hydrochloric acid was added to the filtrate
  18. additionThe resulting solution was added dropwise to 600 ml of acetone
  19. stirringby stirring for 24 hours
  20. temperatureunder cooling with ice
  21. filtrationThen, the precipitate was collected by filtration

出典と根拠

ORDレコード
ord-44b5b86d2d244cf787e609459b05e07b
出典データセット
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05885990

反応ノート

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