Trifluoroacetic acid → 2-Amino-3-methylbutyric acid 2-{[6-(4-bromo-2-chlorophenylamino)-7-fluoro-3-methyl-3H-benzoimidazole-5-carbonyl]-aminooxy}-ethylester hydrochloric acid salt

HRID 1176934ノート

反応式

HRID 1176934 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[C:10]([C:20]([NH:22][O:23][CH2:24][CH2:25][O:26][C:27](=[O:40])[CH:28]([NH:32]C(OC(C)(C)C)=O)[CH:29]([CH3:31])[CH3:30])=[O:21])=[CH:11][C:12]3[N:16]([CH3:17])[CH:15]=[N:14][C:13]=3[C:18]=2[F:19])=[C:4]([Cl:41])[CH:3]=1.FC(F)(F)C(O)=O>>[ClH:41].[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[C:10]([C:20]([NH:22][O:23][CH2:24][CH2:25][O:26][C:27](=[O:40])[CH:28]([NH2:32])[CH:29]([CH3:31])[CH3:30])=[O:21])=[CH:11][C:12]3[N:16]([CH3:17])[CH:15]=[N:14][C:13]=3[C:18]=2[F:19])=[C:4]([Cl:41])[CH:3]=1

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 86592879HCID 86592879、化合物

生成物 1

HCID 865928812-Amino-3-methylbutyric acid 2-{[6-(4-bromo-2-chlorophenylamino)-7-fluoro-3-methyl-3H-benzoimidazole-5-carbonyl]-aminooxy}-ethylester hydrochloric acid salt

実験手順

A mixture of 2-tert-butoxycarbonylamino-3-methylbutyric acid 2-{[6-(4-bromo-2-chlorophenylamino)-7-fluoro-3-methyl-3H-benzoimidazole-5-carbonyl]-aminooxy}-ethylester and its N-acylated isomer (0.6 g) were treated with 1.5 mL of trifluoroacetic acid for 0.5 hours. An HPLC trace of the reaction mixture showed the reaction was complete. The mixture was concentrated on a rotary evaporator and pumped on high vacuum to give yellow oil (0.9 g). The deprotected samples were submitted for HPLC purification to give purified product as a trifluoroacetic acid salt.

後処理

  1. concentrationThe mixture was concentrated on a rotary evaporator

出典と根拠

ORDレコード
ord-b580c3d5340b4e0ca7b0170fc0098f5e
出典データセット
uspto-grants-2010_11
特許番号
US07842816B2

反応ノート

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