反応式
CCN(C(C)C)C(C)C.[CH3:10][C:11]([O:14][C:15]([NH:17][C@H:18]([C:27]([OH:29])=O)[CH2:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[O:16])([CH3:13])[CH3:12].[NH2:30][C@H:31]([C:36]([O:38][CH2:39][C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1)=[O:37])[CH2:32][CH:33]([CH3:35])[CH3:34].CC1C=CC(S(O)(=O)=O)=CC=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.Cl>C(Cl)Cl>[C:11]([O:14][C:15]([NH:17][C@@H:18]([CH2:19][CH2:20][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)[C:27]([NH:30][C@@H:31]([CH2:32][CH:33]([CH3:35])[CH3:34])[C:36]([O:38][CH2:39][C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1)=[O:37])=[O:29])=[O:16])([CH3:10])([CH3:12])[CH3:13]参加物
8
反応物 6
HCID 313Hydrochloric Acid
HCID 6101p-Toluenesulfonic acid
HCID 81531Diisopropylethylamine
HCID 6451313Benzyl L-leucinate
HCID 7018726(2S)-2-(((tert-butoxy)carbonyl)amino)-4-phenylbutanoic acid
HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)生成物 1
試薬・触媒・溶媒 1
実験手順
Referring to FIG. 45, DIPEA (2 mL, 12 mmol, 2.7 eq) was added to a mixture of Boc-HoPhe-OH (1.25 g, 4.4 mmol, 1 eq). H-Leu-OBn.TsOH (1.75 g, 4.5 mmol, 1.0 eq) and HATU (2 g, 5 mmol, 1.1 eq) in CH2Cl2 (50 mL) and the mixture was stirred for four hours at RT. The mixture was poured into 0.5N aq. HCl and extracted twice with CH2Cl2. The combined organic extracts were dried over Na2SO4 and concentrated in vacuo. The residue was purified by chromatography (SiO2, 0-30% EtOAc in heptanes) and product (2.7 g, 100%) was isolated as a colorless oil.
後処理
- extractionextracted twice with CH2Cl2
- dry with materialThe combined organic extracts were dried over Na2SO4
- concentrationconcentrated in vacuo
- customThe residue was purified by chromatography (SiO2, 0-30% EtOAc in heptanes)
出典と根拠
- ORDレコード
- ord-66bf90c18381461b8ec7fc4f78c1ccf0
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09315542B2
関連ノート
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