Hydrochloric Acid → HCID 131713676, 화합물

HRID 648824노트

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HRID 648824 반응식
[C:1]([NH:9][CH:10]([CH2:37][CH2:38][CH2:39][CH2:40][NH:41]C(OCC1C=CC=CC=1)=O)[C:11](=[O:36])[CH2:12][N:13](C(OCC1C=CC=CC=1)=O)[C@H:14]([C:16]([N:18]1[CH2:25][CH2:24][CH2:23][C@H:19]1[C:20]([OH:22])=[O:21])=[O:17])[CH3:15])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:52].Cl.NCCCCC(NC(=O)C1C=CC=CC=1)C(=O)CN[C@H](C(N1CCC[C@H]1C(O)=O)=O)C.CO>C(O)C.[Pd].C(O)CCC.C(O)(=O)C.O>[ClH:52].[ClH:52].[NH2:41][CH2:40][CH2:39][CH2:38][CH2:37][CH:10]([NH:9][C:1](=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:11](=[O:36])[CH2:12][NH:13][C@H:14]([C:16]([N:18]1[CH2:25][CH2:24][CH2:23][C@H:19]1[C:20]([OH:22])=[O:21])=[O:17])[CH3:15]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 53737249HCID 53737249, 화합물HCID 131713678HCID 131713678, 화합물

생성물 1

HCID 131713676HCID 131713676, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 22056973Butanol acetic acid water용매

실험 절차

1-[N-[3-(Benzoylamino)-7-[[(phenylmethoxy)carbonyl]amino]-2-oxoheptyl]-N-[(phenylmethoxy)carbonyl]-L-alanyl]-L-proline, phenylemethyl ester (1.3 g., 1.6 mmole) is dissolved in ethanol (75 ml.) and aqueous hydrochloric acid (1N, 5 ml.). Palladium on carbon catalyst (10%, 450 mg.) is added and the mixture is hydrogenated at atmospheric pressure overnight. The catalyst is filtered off and the solution is evaporated in vacuo. The residue is dissolved in water and lyophilized. The lyophilate is triturated with ether to give 0.6 g. of 1-[N-[7-amino-3-(benzoylamino)-2-oxoheptyl]-L-alanyl]-L-proline, hydrochloride; m.p. 80°-155°; [α]D22 =-50° (c=1.1, methanol). Rf 0.09 (silica gel, n-butanol/acetic acid/water, 4:1:1).

후처리

  1. customis hydrogenated at atmospheric pressure overnight
  2. filtrationThe catalyst is filtered off
  3. customthe solution is evaporated in vacuo
  4. dissolutionThe residue is dissolved in water
  5. customThe lyophilate is triturated with ether
  6. customto give 0.6 g

출처 및 근거

ORD 기록
ord-96660e15163c4d7794678b597d50b001
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04736066

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