. Author manuscript; available in PMC: 2018 Mar 28.

Published in final edited form as: J Labelled Comp Radiopharm. 2017 Jul 25;61(3):252–262. doi: 10.1002/jlcr.3528

Table 1.

“In-loop” formation of [¹¹C]11 and [¹¹C]12



Entry	Benzylamine (8) (μmol)	Trapped [¹¹C]CO₂ (%)^c	RCY of [¹¹C]11 (%)^d	RCY of [¹¹C]12 (%)^d
1^b	4.6	>99	98±1^h	-
2^a	4.6	>99	16	68
3^a	1.3	>99	37	46
4^a	0.6	>99	52	29
5^a	0.3	>99	83±2^h	4
6^a	0.15	>99	70	1
7^a, ^e	0.3	>99	91	4
8^a, ^f	0.3	>99	2	10
9^a, ^g	0.3	>99	13	52

Reaction conditions: Using Route 1, benzylamine (0.15–4.6 μmol), BEMP (2.5 μL, 8.6 μmol), DMF (40 μL), 0.2% POCl₃ (v/v) in MeCN (100 μL, 1.1 μmol), 50% MeOH (v/v) in DMF (50 μL, 1.2 mmol).

Using Route 2, with 10% iodomethane (v/v) in MeCN (100 μL) as alkylating agent.

Percentage [¹¹C]CO₂ left in loop after entrapment.

Non-isolated radiochemical yield (RCY), based on radio-HPLC analysis of the crude product.

MeCN was used as solvent.

DMSO was used as solvent.

DBU was used as fixation base.

(n = 3); all other entries unless noted represent single experiments.