Trifluoroacetic acid → HCID 86692460, 화합물

반응식

[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2([C:18]#[N:19])[CH2:17][CH2:16][C:11]3(OCC[O:12]3)[CH2:10][CH2:9]2)=[N:6][CH:7]=1.FC(F)(F)C(O)=O>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2([C:18]#[N:19])[CH2:9][CH2:10][C:11](=[O:12])[CH2:16][CH2:17]2)=[N:6][CH:7]=1

참가 물질

반응물 2

HCID 6422Trifluoroacetic acid

HCID 86692457HCID 86692457, 화합물

생성물 1

HCID 86692460HCID 86692460, 화합물수율 94.7%

실험 절차

To 8-(5-bromopyridin-2-yl)-1,4-dioxaspiro[4.5]decane-8-carbonitrile (3.4 g) described in Reference Example 82 was added trifluoroacetic acid (4.1 ml) at room temperature, and stirred at the same temperature for 22 hours. After completion of the reaction, the solvent and trifluoroacetic acid were evaporated. The obtained residue was purified with silica gel column chromatography (n-hexane:ethyl acetate) to give 1-(5-bromopyridin-2-yl)-4-oxocyclohexanecarbonitrile (2.78 g) as a white solid.

후처리

customAfter completion of the reaction
customthe solvent and trifluoroacetic acid were evaporated
customThe obtained residue was purified with silica gel column chromatography (n-hexane:ethyl acetate)

출처 및 근거

ORD 기록: ord-02ca3153db0340a9b9392d8df166cde7
출처 데이터셋: uspto-grants-2015_10
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09150555B2

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