Trifluoroacetic acid → IDN-1965

HRID 2120631ノート

反応式

HRID 2120631 の反応式
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([CH3:11])=[C:3]1[C:12]([NH:14][C@H:15]([C:19]([NH:21][CH:22]([C:31](=[O:34])[CH2:32][F:33])[CH2:23][C:24]([O:26]C(C)(C)C)=[O:25])=[O:20])[CH:16]([CH3:18])[CH3:17])=[O:13].FC(F)(F)C(O)=O>C1(OC)C=CC=CC=1.C(Cl)Cl>[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([CH3:11])=[C:3]1[C:12]([NH:14][C@H:15]([C:19]([NH:21][CH:22]([C:31](=[O:34])[CH2:32][F:33])[CH2:23][C:24]([OH:26])=[O:25])=[O:20])[CH:16]([CH3:17])[CH3:18])=[O:13]

参加物

5

反応物 2

HCID 6422Trifluoroacetic acidHCID 86584477HCID 86584477、化合物

生成物 1

HCID 9802179IDN-1965収率 48.2%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 7519Anisole溶媒

実験手順

A solution of N-[(1,3-dimethylindole-2-carbonyl)valinyl]-3-amino-4-oxo-5-fluoropentanoic acid, t-butyl ester (40 mg) in anisole (0.2 mL) and methylene chloride (2 mL) was treated with trifluoroacetic acid (1 mL), and the resultant reaction mixture was stirred for 30 minutes under a nitrogen atmosphere at room temperature. The reaction mixture was concentrated and chased with methylene chloride to give a solid. The solid was triturated with ether to yield the title product as a brown powder (17 mg). TLC: (methylene chloride/methanol/acetic acid, 20:1:1): Rf=0.40. MS (EI) for C12H26FN3O5: MH+=420; MH−=418.

後処理

  1. customthe resultant reaction mixture
  2. concentrationThe reaction mixture was concentrated
  3. customto give a solid
  4. customThe solid was triturated with ether

出典と根拠

ORDレコード
ord-ef327a14394b4be2ad71d3d33f3f8904
出典データセット
uspto-grants-2004_02
特許番号
US06693096B2

反応ノート

読み込み中…