Toluene → HCID 66863531、化合物

関与物質

役割	名称	HCID	仕込み量
反応物	Toluene	HCID 1140	—
反応物	(2R,3S)-1-tert-Butyloxycarbonyl-3-(tert-butyldimethylsilanyloxy)-2-[(1S)-1-(3-chloro-4-cyano-2-methyl-phenylamino)ethyl]pyrrolidine	HCID 16732285	—
溶媒	Dichloromethane	HCID 6344	—
溶媒	Trifluoroacetic acid	HCID 6422	—
生成物	HCID 66863531	HCID 66863531	56.4%

反応手順

Intermediate 61H (825 mg, 1.67 mmol) was dried azeotropically with toluene (2×). The residue was taken up in 15% TFA in CH2Cl2 (10 mL) and stirred at rt for 5 h. Toluene (10 mL) was added and solvent was removed under vacuum. The product was purified by reverse phase HPLC (Phenoenex Luna 30×100 mm S5 C18, 10 min. grad, 25 mL/min, 20-100% B solvent, A=10% MeOH/water+0.1% TFA, B=90% MeOH/Water+0.1% TFA, 4 injections). Solvent was reduced to ˜10% volume and the product was then extracted into EtOAc, washed with sat. aqueous NaHCO3, dried over MgSO4 and filtered. Solvents were removed to provide the title compound (371 mg): MS (ES) m/z 394.53 [M+H]+

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07405234B2
出典データセット	uspto-grants-2008_07
ORD ID	ord-7d57bd5f340c4eb88090cc7d1eb7a871
出典メモ	uspto-grants-2008_07