Trifluoroacetic acid → HCID 178520673、化合物

HRID 2289078ノート

反応式

HRID 2289078 の反応式
[N+:1]([C:4]1[CH:48]=[CH:47][C:7]([CH2:8][O:9][C:10]([N:12]=[C:13]([NH:33][C:34]([O:36][CH2:37][C:38]2[CH:43]=[CH:42][C:41]([N+:44]([O-:46])=[O:45])=[CH:40][CH:39]=2)=[O:35])[NH:14][CH2:15][CH2:16][CH2:17][C:18]([NH:20][C@H:21]2[CH2:25][CH2:24][N:23](C(OC(C)(C)C)=O)[CH2:22]2)=[O:19])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].[F:49][C:50]([F:55])([F:54])[C:51]([OH:53])=[O:52]>ClCCl.ClCCCl>[F:49][C:50]([F:55])([F:54])[C:51]([OH:53])=[O:52].[N+:1]([C:4]1[CH:48]=[CH:47][C:7]([CH2:8][O:9][C:10]([N:12]=[C:13]([NH:33][C:34]([O:36][CH2:37][C:38]2[CH:43]=[CH:42][C:41]([N+:44]([O-:46])=[O:45])=[CH:40][CH:39]=2)=[O:35])[NH:14][CH2:15][CH2:16][CH2:17][C:18]([NH:20][C@H:21]2[CH2:25][CH2:24][NH:23][CH2:22]2)=[O:19])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

5

反応物 2

HCID 6422Trifluoroacetic acidHCID 178452033HCID 178452033、化合物

生成物 1

HCID 178520673HCID 178520673、化合物

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of the compound (2.50 g), which had been obtained in (1), in anhydrous dichloromethane (25 ml), trifluoroacetic acid (15 ml) was added dropwise under ice cooling, followed by stirring at the same temperature for 15 minutes and at room temperature for 15 minutes. The reaction mixture was diluted with 1,2-dichioroethane and concentrated by evaporation under reduced pressure. The residue was washed successively with hexane and diethyl ether by decantation and then the solvent was distilled off, whereby crude (3S)-3-[4-[2,3,-di(4-nitrobenzyloxycarbonyl)guanidino]butanoylamino]pyrrolidine trifluoroacetate (2.55 g) was obtained. The product was provided for use in the subsequent reaction without isolation.

後処理

  1. concentrationconcentrated by evaporation under reduced pressure
  2. washThe residue was washed successively with hexane and diethyl ether by decantation
  3. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-13893cf886cd44e28fbf0e16b8bb6ec2
出典データセット
uspto-grants-2000_07
特許番号
US06090802

反応ノート

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