Acetonitrile → HCID 59865001、化合物

温度

30 °C

A mixture of 1-[(3-chloropropyl)oxy]-4-iodobenzene (100 g) and acetonitrile (600 ml) is stirred for about 5 min at 25-35° C., then potassium carbonate (93.07 g) followed by 3,3-dimethylpiperidine (49.53 g) are added over about 10 min. Potassium iodide (2.24 g) is added, then the mixture is stirred for about 15 min, before being heated to 78-82° C. for 22-24 h. The reaction mixture is cooled to 25-35° C., and the solid residue is filtered and washed with acetonitrile (200 ml). The filtrate and washings are concentrated under reduced pressure at 50-60° C. to give a thick liquid which is stirred with n-heptane (100 ml) for about 30 min at 25-30° C. The solution is then cooled to −5 to 10° C. and stirred for about 30 min. The solid is filtered, washed with chilled n-heptane (50 ml, 0-5° C.), then dried at 35-40° C. under vacuum for 6-10 h to give the title compound (97 g).

1. additionare added over about 10 min
2. stirringthe mixture is stirred for about 15 min
3. temperaturebefore being heated to 78-82° C. for 22-24 h
4. temperatureThe reaction mixture is cooled to 25-35° C.
5. filtrationthe solid residue is filtered
6. washwashed with acetonitrile (200 ml)
7. concentrationThe filtrate and washings are concentrated under reduced pressure at 50-60° C.
8. customto give a thick liquid which
9. temperatureThe solution is then cooled to −5 to 10° C.
10. stirringstirred for about 30 min
11. filtrationThe solid is filtered
12. washwashed with chilled n-heptane (50 ml, 0-5° C.)
13. customdried at 35-40° C. under vacuum for 6-10 h

ORDレコード

ord-a900d12195054f1d9fb2ae45e4a9e19a

出典データセット

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07989629B2