Diisopropylethylamine → HCID 86612926、化合物
反応式
FC(F)(F)C(O)=O.[NH2:8][CH:9]1[CH2:13][CH:12]([OH:14])[CH:11]([OH:15])[CH2:10]1.CCN(C(C)C)C(C)C.[N:25]1([C:31]([NH:33][C@@H:34]([CH2:38][S:39]([CH2:42][C:43]2[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=2)(=[O:41])=[O:40])[C:35](O)=[O:36])=[O:32])[CH2:30][CH2:29][O:28][CH2:27][CH2:26]1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C>[OH:15][CH:11]1[CH:12]([OH:14])[CH2:13][CH:9]([NH:8][C:35]([C@@H:34]([NH:33][C:31]([N:25]2[CH2:30][CH2:29][O:28][CH2:27][CH2:26]2)=[O:32])[CH2:38][S:39]([CH2:42][C:43]2[CH:44]=[CH:45][CH:46]=[CH:47][CH:48]=2)(=[O:41])=[O:40])=[O:36])[CH2:10]1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
A solution of 4-amino-cyclopentane-1,2-diol; compound with trifluoroacetic acid (745 mg, 3.23 mmol) in DMF (15 ml) was treated with DIPEA (1.12 ml, 6.4 mmol) and the mixture was stirred for 5 minutes at room temperature. Then (R)-2-[(Morpholine-4-carbonyl)-amino]-3-phenylmethanesulfonyl-propionic acid (1.15 g, 3.23 mmol) was added followed by HATU (1.23 g, 3.24 mmol). This mixture was stirred at room temperature overnight and then evaporated. The residue was subjected to flash chromatography on silica eluting with ethyl acetate and then with a mixture of ethyl acetate and methanol to give morpholine-4-carboxylic acid [(R)-1-(3,4-dihydroxy-cyclopentylcarbamoyl)-2-phenylmethanesulfonyl-ethyl]-amide as a brown solid (680 mg). LC/MS: RT=2.64 min. (215 and 254 nM), MH+=456.
後処理
- stirringThis mixture was stirred at room temperature overnight
- customevaporated
- additionwith a mixture of ethyl acetate and methanol
出典と根拠
- ORDレコード
- ord-b15e9185bd194491af69548d2bd8388f
- 出典データセット
- uspto-grants-2007_03
- 特許番号
- US07196099B2
反応ノート
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