Dicyclohexylcarbodiimide → HCID 178479473, 화합물

HRID 358266

반응식

HRID 358266 반응식
[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]

참가 물질

5

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 11349FlavonolHCID 178479474HCID 178479474, 화합물

생성물 1

HCID 178479473HCID 178479473, 화합물수율 5.2%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7c349e4ebb7b407ebf4351ff1f3fb8a9
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04465851

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