반응 #837217

반응 방정식

product

(R)-2-[4-(2,4-Dichloro-benzyloxy)-phenoxymethyl]-pyrrolidine-1-carboxylic acid tert-butyl ester

HCl

ether

→

title product

(R)-2-[4-(2,4-Dichloro-benzyloxy)-phenoxymethyl]-pyrrolidine hydrogen chloride salt

용매

MeOH

반응 조건

후처리

1. 1
   기타the solid which formed
2. 2
   여과was filtered out
3. 3
   기타to provide the crude which
4. 4
   기타was further purified by recrystallization with MeOH-ether

실험 절차

To a 25 mL vial which contained a solution of the product from step 2 (120 mg, 0.26 mmol) in MeOH (2 mL) was added HCl (2 N in ether, 4 mL) at 0° C. The mixture was allowed to warm to rt and stir at rt for 24 h. The ether (10 mL) was added to the mixture and the solid which formed was filtered out to provide the crude which was further purified by recrystallization with MeOH-ether to yield the title product, (104 mg, 95%); LCMS; 100% APCI+, Calcd: 352.3. Found m/z 352.3 (M). 1H NMR (400 MHz, DMSO-d6); δ 1.68-1.75 (m, 1H), 1.84-2.02 (m, 2H), 2.07-2.16 (m, 1H), 3.13-3.26 (m, 2H), 3.80-3.90 (m, 1H), 4.05-4.10 (m, 1H), 4.18 (dd, J1=10.4 Hz, J2=3.6 Hz, 1H), 5.09 (s, 2H), 6.94-7.01 (m, 4H), 7.48 (dd, J1=8.0 Hz, J2=2.0 Hz, 1H), 7.60 (d, J=8.4 Hz, 1H), 7.68 (d, 1H, J=2.0 Hz):

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