17-{3-[(2-Benzyloxycarbonylethyl)tert-butoxycarbonylamino]propionylamino}heptadecanoic acid tert-butyl ester → 17-{3-[tert-Butoxycarbonyl (2-carboxyethyl)amino]propionylamino}heptadecanoic acid tert-butyl ester
反応式
[C:1]([O:5][C:6](=[O:48])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][NH:23][C:24](=[O:47])[CH2:25][CH2:26][N:27]([CH2:35][CH2:36][C:37]([O:39]CC1C=CC=CC=1)=[O:38])[C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])([CH3:4])([CH3:3])[CH3:2]>C1COCC1>[C:1]([O:5][C:6](=[O:48])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][NH:23][C:24](=[O:47])[CH2:25][CH2:26][N:27]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:35][CH2:36][C:37]([OH:39])=[O:38])([CH3:4])([CH3:2])[CH3:3]参加物
3
実験手順
17-{3-[(2-Benzyloxycarbonylethyl)tert-butoxycarbonylamino]propionylamino}heptadecanoic acid tert-butyl ester (0.135 g, 0.2 mmol) was dissolved in THF (10 mL) in a flask. The flask was filled with nitrogen and purged under vacuum several times. Pd/C, wet 10% (0.03 g) was added and the flask was equipped with a balloon filled with the mixture was stirred for 16 h. The mixture was filtered through a celite, eluting with THF. The filtrate was concentrated under vacuum. TLC indicated the reaction was not complete, so the process was repeated twice more. The filtrate was concentrated under vacuum to yield a yellow oil (0.12 g)
後処理
- additionThe flask was filled with nitrogen
- custompurged under vacuum several times
- additionPd/C, wet 10% (0.03 g) was added
- customthe flask was equipped with a balloon
- additionfilled with the mixture
- filtrationThe mixture was filtered through a celite
- washeluting with THF
- concentrationThe filtrate was concentrated under vacuum
- concentrationThe filtrate was concentrated under vacuum
出典と根拠
- ORDレコード
- ord-a56a7a4af1394f78af270315569bf34c
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08710000B2
反応ノート
読み込み中…