2,4,6-Trimethylpyridine → 3-{[5-(3-tert-Butoxycarbonylamino-propylcarbamoyl)-thiophene-2-carbonyl]-amino}-3-phenyl-propionic Acid Tert-butyl Ester
反応式
[C:1]([O:5][C:6]([NH:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]([C:15]1[S:19][C:18]([C:20]([OH:22])=O)=[CH:17][CH:16]=1)=[O:14])=[O:7])([CH3:4])([CH3:3])[CH3:2].[C:23]([O:27][C:28](=[O:38])[CH2:29][CH:30]([NH2:37])[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)([CH3:26])([CH3:25])[CH3:24].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.N1C(C)=CC(C)=CC=1C>CN(C=O)C.C(OCC)(=O)C.CCCCCC>[C:23]([O:27][C:28](=[O:38])[CH2:29][CH:30]([NH:37][C:20]([C:18]1[S:19][C:15]([C:13](=[O:14])[NH:12][CH2:11][CH2:10][CH2:9][NH:8][C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])=[CH:16][CH:17]=1)=[O:22])[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)([CH3:26])([CH3:24])[CH3:25]参加物
7
反応物 4
HCID 79532,4,6-Trimethylpyridine
HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
HCID 14557402Tert-butyl 3-amino-3-phenylpropanoate
HCID 222852255-(3-tert-Butoxycarbonylamino-propylcarbamoyl)-thiophene-2-carboxylic Acid生成物 1
試薬・触媒・溶媒 2
実験手順
With continued reference to Scheme G, 5-(3-tert-Butoxycarbonylamino-propylcarbamoyl)-thiophene-2-carboxylic acid (200 mg, 0.704 mmol) was reacted with 3-Amino-3-phenyl-propionic acid tert-butyl ester (187 mg, 0.845 mmol) in 4.0 ml of anhydrous DMF using HATU (321 mg, 0.845 mmol) with 2,4,6-collidine (0.25 ml, 2.112 mmol), chromatographied on silica gel using ethyl acetate: hexane (8:2) to give 200 mg (58% yield) of the desired product as a clear semi-solid oil. 1H NMR (400 Mhz, CDCl3) 1.3 (s, 9H), 1.45 (s, 9H), 1.7 (m, 2H), 2.9 (ddd, 2H), 3.25 (m, 2H), 3.5 (q, 2H), 4.85 (bs, 1H), 5.55 (m, 1H), 7.23 (m, 1H), 7.33 (m, 4H), 7.4-7.6 (m, 4H).
出典と根拠
- ORDレコード
- ord-e4ff4c47a8334334a6bbf207a556f226
- 出典データセット
- uspto-grants-2005_11
- 特許番号
- US06960594B2
反応ノート
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