Diisobutylaluminum hydride → HCID 89556341、化合物

温度

-10 °C

1-(4,6-Dichloro-3-pyridyl)cyclopropanecarbonitrile (0.1 g, 0.469 mmol) was dissolved in Toluene (2.3 mL). At −10° C. DIBAL-H 1M in Toluene (0.98564 mL, 0.986 mmol) was added dropwise. The reaction mixture was stirred 30 min at −10° C. At −10° C. NaBH4 (0.10871 g, 2.816 mmol) was added, then carefully 3 mL MeOH. The reaction mixture was stirred 30 min at rt. It was poured into 25 ml of 1N potassium sodium tartrate. The pale yellow solution was extracted 3 times with Ether. The combined organic phases were washed with brine and dried with Na2SO4, filtrated and the filtrate evaporated. The product was obtained as a pale yellow oil (99 mg).

1. customAt −10° C
2. customAt −10° C
3. stirringThe reaction mixture was stirred 30 min at rt
4. extractionThe pale yellow solution was extracted 3 times with Ether
5. washThe combined organic phases were washed with brine
6. dry with materialdried with Na2SO4
7. filtrationfiltrated
8. customthe filtrate evaporated

ORDレコード

ord-04d8bf1bce4d45f7b1e5d985f6d6de7d

出典データセット

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09040708B2