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Pyridine → HCID 178486235、化合物

HRID 1419237
ノート
印刷プレビュー

反応式

HRID 1419237 の反応式
N1C=CC=CC=1.[ClH:7].[CH3:8][NH:9][N:10]=[CH:11][NH:12][C:13]1[CH:21]=[CH:20][C:16]([C:17]([OH:19])=[O:18])=[CH:15][CH:14]=1.Cl.[C:23]([C:26]1[CH:27]=[C:28]2[C:33](=[CH:34][CH:35]=1)[C:32]([CH2:36][C:37](=[O:39])[NH2:38])=[C:31](O)[CH:30]=[CH:29]2)(=[NH:25])[NH2:24].C1CCC(N=C=NC2CCCCC2)CC1>CN(C1C=CN=CC=1)C.C(C(C)=O)C.O.C(O)(=O)C>[ClH:7].[ClH:7].[CH3:8][NH:9][N:10]=[CH:11][NH:12][C:13]1[CH:21]=[CH:20][C:16]([C:17]([O:19][C:31]2[CH:30]=[CH:29][C:28]3[C:33](=[CH:34][CH:35]=[C:26]([C:23](=[NH:24])[NH2:25])[CH:27]=3)[C:32]=2[CH2:36][C:37](=[O:39])[NH2:38])=[O:18])=[CH:15][CH:14]=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 1049PyridineHCID 10868DicyclohexylcarbodiimideHCID 1364542706-Amidino-1-carbamoylmethyl-2-naphthol.hydrochlorideHCID 178486236HCID 178486236、化合物

生成物 1

HCID 178486235HCID 178486235、化合物収率 103%

試薬・触媒・溶媒 2

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 131721204Methyl ethyl ketone acetic acid water溶媒

実験手順

20 Milliliters of 20% hydrous pyridine was added to 600 mg of 4-methylaminoiminomethylaminobenzoic acid.hydrochloride, 730 mg of 6-amidino-1-carbamoylmethyl-2-naphthol.hydrochloride, 646 mg of DCC and 32 mg of DMAP, followed by stirring for 2 hours under cooling with ice and then 48 hours at room temperature. The precipitate was filtered and the filtrate was concentrated under reduced pressure. To the residue was added 20 ml of DMF, and the solution was added dropwise to 300 ml of acetone, followed by stirring for 24 hours under cooling with ice. Then, the precipitate was collected by filtration to obtain a crude product. Then, the product was subjected to silica gel column chromatography using methyl ethyl ketone-water-acetic acid (80:15:5) as an eluent, and the desired fractions were collected and the solvent was distilled off under reduced pressure. To the residue were added 15 ml of methanol and 440 μl of concentrated hydrochloric acid, and the solution was added dropwise to a mixed liquid of 300 ml of acetone and 100 ml of ether, followed by stirring for 24 hours under cooling with ice. Then, the precipitate was collected by filtration to obtain 661.1 mg of the desired product.

後処理

  1. temperatureunder cooling with ice
  2. custom48 hours
  3. customat room temperature
  4. filtrationThe precipitate was filtered
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. additionTo the residue was added 20 ml of DMF
  7. additionthe solution was added dropwise to 300 ml of acetone
  8. stirringby stirring for 24 hours
  9. temperatureunder cooling with ice
  10. filtrationThen, the precipitate was collected by filtration
  11. customto obtain a crude product
  12. customthe desired fractions were collected
  13. distillationthe solvent was distilled off under reduced pressure
  14. additionTo the residue were added 15 ml of methanol and 440 μl of concentrated hydrochloric acid
  15. additionthe solution was added dropwise to a mixed liquid of 300 ml of acetone and 100 ml of ether
  16. stirringby stirring for 24 hours
  17. temperatureunder cooling with ice
  18. filtrationThen, the precipitate was collected by filtration

出典と根拠

ORDレコード
ord-df3f0fb29c0540689cd26b496fd583f6
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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