Trifluoroacetic acid → HCID 89719307、化合物

HRID 63727

反応式

HRID 63727 の反応式
[CH3:1][O:2][C:3](=[O:46])[C@@H:4]([NH:23][C:24](=[O:45])[C:25]1[C:30]([Cl:31])=[CH:29][C:28]([O:32][CH2:33][CH2:34][CH2:35][NH:36]C(OC(C)(C)C)=O)=[CH:27][C:26]=1[Cl:44])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([NH:12][C:13](=[O:22])[C:14]2[C:19]([Cl:20])=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:21])=[CH:8][CH:7]=1.C(O)(C(F)(F)F)=O>ClCCl>[CH3:1][O:2][C:3](=[O:46])[C@@H:4]([NH:23][C:24](=[O:45])[C:25]1[C:26]([Cl:44])=[CH:27][C:28]([O:32][CH2:33][CH2:34][CH2:35][NH2:36])=[CH:29][C:30]=1[Cl:31])[CH2:5][C:6]1[CH:7]=[CH:8][C:9]([NH:12][C:13](=[O:22])[C:14]2[C:19]([Cl:20])=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:21])=[CH:10][CH:11]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 89717547(S)-2-[4-(3-tert-butoxycarbonylaminopropoxy)-2,6-dichlorobenzoylamino]-3-[4-(2,6-dichlorobenzoylamino)phenyl]propionic acid methyl ester

生成物 1

HCID 89719307HCID 89719307、化合物収率 118.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of (S)-2-[4-(3-tert-butoxycarbonylaminopropoxy)-2,6-dichlorobenzoylamino]-3-[4-(2,6-dichlorobenzoylamino)phenyl]propionic acid methyl ester (7.5 g, 7.98 mmol) in dichloromethane (100 mL) was added an excess of TFA (9.12 g, 5.9 mL, 80 mmol) at room temperature. The resulting solution was stirred for 15 h. Then, the solvent was removed under vacuum and the residue was azeotrophed one time with toluene. After drying under high vacuum, 5.8 g (99%) of (S)-2-[4-(3-aminopropoxy)-2,6-dichlorobenzoylamino]-3-[4-(2,6-dichlorobenzoylamino)phenyl]propionic acid methyl ester was obtained as a white solid. ES(+)-HRMS m/e calcd. for C27H25Cl4N3O5 (M+H)+ 612.0621, obsd. 612.0619.

後処理

  1. customThen, the solvent was removed under vacuum
  2. customAfter drying under high vacuum

出典と根拠

ORDレコード
ord-c51cf0cc9a4948cf95c67713976f5da1
出典データセット
uspto-grants-2016_09
特許番号
US09447035B2

関連ノート

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