Table 2. The reaction scope ^a .

Entry	R	R1	t/h	Yield of 3 (%)	NMR yield of [4 + 5] b (%)
1	H (1a)	TMS (2a)	2	68 (3aa)	11
2 c	H (1a)	TMS (2a)	2	62 (3aa)	N.D. d
3	4-Me (1b)	TMS (2a)	2	57 (3ba)	10
4	4- t Bu (1c)	TMS (2a)	2	47 (3ca) e	8
5	4-OMe (1d)	TMS (2a)	2	55 (3da)	10
6	4-CO2Me (1e)	TMS (2a)	2.5	60 (3ea)	10
7	4-Cl (1f)	TMS (2a)	2	50 (3fa)	10
8	4-Br (1g)	TMS (2a)	2	50 (3ga)	11
9	4-CF3 (1h)	TMS (2a)	3	53 (3ha)	11
10	4-NO2 (1i)	TMS (2a)	12	62 (3ia)	7
11	2-Me (1j)	TMS (2a)	48	23 (3ja)	8
12	H (1a)	Ph (2b)	5	56 (3ab) f	N.D.
13	H (1a)	p-ClC6H4 (2c)	18	63 (3ac) g	N.D.
14	H (1a)	p-MeOC6H4 (2d)	10	45 (3ad) h	N.D.
15 i	H (1a)	3-Thienyl (2e)	48	47 (3ae) j	N.D.
16 k	H (1a)	Bu (2f)	14	34 (3af)	N.D.

^aThe reaction was conducted with 1 (1 mmol), 2 (1 mmol), [Cp*RhCl₂]₂ (0.02 mmol), K₂CO₃ (0.3 mmol) and MeOH (6 mL), and monitored by TLC.

^bDetermined by ¹H NMR using dibromomethane as internal standard.

^cReaction was conducted on 6 mmol scale.

^dNot determined.

^e97% purity.

^f94% purity.

^g92% purity.

^h91% purity.

ⁱReaction was conducted at 55 °C.

^j90% purity.

^k 1a (1.5 mmol), 2f (1 mmol) and [Cp*RhCl₂]₂ (0.04 mmol) were used.