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. 2021 Dec 24;24(1):27–32. doi: 10.1021/acs.orglett.1c03569

Table 1. Optimization of Reaction Conditionsa.

graphic file with name ol1c03569_0006.jpg

entry variation from initial conditionsa yieldb (%)
1 none 62
2 0.16 M instead of 0.08 M 47c
3 5 h instead of 3 h 20
4 4 Å MS as an additive 53
5 AgPF6 (1.5 equiv) as an additive 23d
6 TFA (1:4 v/v with THF) as an additive 25d
7 TEMPO (10 mol %) as an additive 25d
8 MeCN instead of THF 37e
9 DMF instead of THF 38
10 CH2Cl2 instead of THF 55
11 MeOH/THF(1:1v/v, 0.08 M) 91
12 without current nr
a

Initial conditions: undivided cell, Pt cathode, C-SK50 anode, constant current = 10 mA, 1 (0.4 mmol), nBu4PF6 (1.0 equiv), MeOH (10 equiv), THF (0.08 M), rt, 3 h.

b

Isolated yield.

c

50% conversion.

d

Partial decomposition was observed.

e

59% conversion.