Dicyclohexylcarbodiimide → HCID 178479473、化合物

HRID 358266

反応式

HRID 358266 の反応式
[ClH:1].[NH:2]([CH2:6][C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([OH:15])=[O:14])[CH2:9][CH2:8]1)[C:3]([NH2:5])=[NH:4].O[C:17]1[C:26](=[O:27])[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[O:19][C:18]=1[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.C1(N=C=NC2CCCCC2)CCCCC1>N1C=CC=CC=1>[ClH:1].[NH:2]([CH2:6][C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([O:15][C:30]2[CH:29]=[C:28]([CH:33]=[CH:32][CH:31]=2)[C:18]2[O:19][C:20]3[C:25]([C:26](=[O:27])[CH:17]=2)=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:14])[CH2:9][CH2:8]1)[C:3]([NH2:5])=[NH:4]

参加物

5

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 11349FlavonolHCID 178479474HCID 178479474、化合物

生成物 1

HCID 178479473HCID 178479473、化合物収率 5.2%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 9.89 g of trans-4-guanidinomethylcyclohexanecarboxylic acid hydrochloride, 10.1 g of 3-hydroxyflavon and 8.66 g of dicyclohexylcarbodiimide was added to 100 ml of dry pyridine, and the resulting mixture was stirred at room temperature for 16 hours. The reaction mixture was filtered to remove any insoluble materials which were washed with pyridine. The filtrate and the washing were combined and evaporated. 0.1N hydrochloric acid was added to the residue, and the mixture was washed with ethyl acetate. The aqueous layer was concentrated to 30 ml and allowed to stand overnight in a refrigerator to obtain 1 g of 3'-flavonyl trans-4-guanidinomethylcyclohexanecarboxylate hydrochloride as colorless needles having a melting point of 201°-203° C.

後処理

  1. filtrationThe reaction mixture was filtered
  2. customto remove any insoluble materials which
  3. washwere washed with pyridine
  4. customevaporated
  5. addition0.1N hydrochloric acid was added to the residue
  6. washthe mixture was washed with ethyl acetate
  7. concentrationThe aqueous layer was concentrated to 30 ml
  8. waitto stand overnight in a refrigerator

出典と根拠

ORDレコード
ord-7c349e4ebb7b407ebf4351ff1f3fb8a9
出典データセット
uspto-grants-1984_08
特許番号
US04465851

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