反応式
[NH2:1][CH2:2][C:3]([OH:5])=O.[NH2:6][C@H:7]([C:12]([OH:14])=O)[C@H:8]([CH2:10][CH3:11])[CH3:9].[NH2:15][C@H:16]([C:20]([OH:22])=O)[C@@H:17]([CH3:19])[OH:18].[NH2:23][C@H:24]([C:28]([OH:30])=[O:29])[CH:25]([CH3:27])[CH3:26].[NH2:31][C@H:32]([C:43]([OH:45])=O)[CH2:33][C:34]1[C:42]2[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=2)[NH:36][CH:35]=1>>[NH2:1][CH2:2][C:3]([NH:31][CH2:32][C:43]([NH:6][C@H:7]([C:12]([NH:31][C@H:32]([C:43]([NH:15][C@H:16]([C:20]([NH:1][C@H:2]([C:3]([NH:23][C@H:24]([C:28]([OH:30])=[O:29])[CH:25]([CH3:27])[CH3:26])=[O:5])[CH2:33][C:34]1[C:42]2[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=2)[NH:36][CH:35]=1)=[O:22])[C@@H:17]([CH3:19])[OH:18])=[O:45])[CH2:33][C:34]1[C:42]2[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=2)[NH:36][CH:35]=1)=[O:14])[C@H:8]([CH2:10][CH3:11])[CH3:9])=[O:45])=[O:5]参加物
実験手順
655 mg of the peptide-resin was treated with 1 mL of anisole and 10 mL of HF for one hour at 0° to 4° C. The HF was removed by nitrogen stream and the resultant solids were triturated with diethyl ether (30 mL). The solids were collected by filtration, washed with diethyl ether (3 ×10 mL) and then extracted with 70% acetic acid (3×10 mL). The extracts were combined and lyophilized to yield 128 mg of crude peptide. 84 mg of the crude peptide had the Trp residues deformylated by dissolution in 2% piperidine (10 mL) and stirring for 2 hours at room temperature. This solution was injected over three runs onto a Vydac 22×250 mm C18 10 μm particle sized 300 Angstrom pore packed column. Elution with a gradient of 30% to 50% B over 30 minutes at a flow rate of 10 mL/min was carried out (Solvent A= 0.1% TFA; Solvent B=0.1% TFA in 80% Ethanol/Water). Fractions were collected and the appropriate ones pooled to give 53 mg of white solid. Amino Acid Analysis: Gly 2.00 (2.00) , Ile 0.92 (1.00) , Thr 0.90 (1.00), Val 1.00 (1.00), Trp 1.79 (2.00), 61% peptide FAB/MS: MH+=818 (MW=817)
出典と根拠
- ORDレコード
- ord-45ab63badfda464f8af76e7623cea03c
- 出典データセット
- uspto-grants-1995_11
- 特許番号
- US05464935
関連ノート
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