Hydrochloric Acid → HCID 131713676、化合物

HRID 648824ノート

反応式

HRID 648824 の反応式
[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]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 53737249HCID 53737249、化合物HCID 131713678HCID 131713678、化合物

生成物 1

HCID 131713676HCID 131713676、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 22056973Butanol acetic acid water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-96660e15163c4d7794678b597d50b001
出典データセット
uspto-grants-1988_04
特許番号
US04736066

反応ノート

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