反応式
CO.C([CH:10]([OH:34])[CH2:11][O:12][CH2:13][CH2:14][O:15][CH2:16][CH2:17][O:18][CH2:19][CH2:20][O:21][CH2:22][CH2:23][O:24][CH2:25][CH2:26][O:27][CH2:28][CH2:29][O:30][CH2:31][CH2:32][OH:33])C1C=CC=CC=1.CCCCCC>[Pd].CC(OC)(C)C>[CH2:32]([OH:33])[CH2:31][O:30][CH2:29][CH2:28][O:27][CH2:26][CH2:25][O:24][CH2:23][CH2:22][O:21][CH2:20][CH2:19][O:18][CH2:17][CH2:16][O:15][CH2:14][CH2:13][O:12][CH2:11][CH2:10][OH:34]参加物
実験手順
10% Pd/C (11.2 g) was added to MeOH (50 mL) at −15° C. in hydrogenation bottle under agron. BnO-dPEG8-OH (69.0 g, 0.15 mole) was added to the bottle along with MeOH (150 mL). The bottle was placed on the Parr shaker for 17 h at 50 psi of H2. The reaction was monitored by tlc on silica gel plates, eluting with 10% MeOH/CH2Cl2. The reaction is about 50% complete. The reaction was worked up. The reaction mixture was filter through glass fiber, used MeOH as needed to make a clean transfer. The filtrate was concentrated in vacuo to give an oil. A column was prepared with 600 g of silica gel and hexane. The crude product was placed onto column with hexane and minimum of TBME (100 mL). The column was eluted as follows: (2 L) 20% TBME/hexane; (2 L) 50% TBME/hexane; (4 L) TBME; (2 L) 5% MeOH/TBME; (2 L) 10% MeOH/TBME. Like fractions containing product were combined and concentrated in vacuo to give 28.5 g (51% yield). The product was characterized by nmr.
後処理
- washeluting with 10% MeOH/CH2Cl2
- filtrationThe reaction mixture was filter through glass fiber
- concentrationThe filtrate was concentrated in vacuo
- customto give an oil
- washThe column was eluted
- additionLike fractions containing product
- concentrationconcentrated in vacuo
- customto give 28.5 g (51% yield)
出典と根拠
- ORDレコード
- ord-12e246cbc2a14362b5f102cc51f2be3c
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07888536B2
関連ノート
読み込み中…