Tetrahydrofuran → HCID 58409945、化合物

HRID 1844916ノート

反応式

HRID 1844916 の反応式
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]1[C:23]2[CH2:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:15]=2[C:14]([C:24]#[N:25])=[C:13]([N:26]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]2)[CH:12]=1.[H-].[Na+].C1C[O:37]CC1>>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]1[C:23]2[C:22](=[O:37])[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:15]=2[C:14]([C:24]#[N:25])=[C:13]([N:26]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]2)[CH:12]=1

参加物

4

反応物 3

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 58409942HCID 58409942、化合物

生成物 1

HCID 58409945HCID 58409945、化合物

反応条件

温度
2.5 °C

実験手順

A solution of 1-(naphthalen-2-yl)-3-(piperidin-1-yl)-9H-fluorene-4-carbonitrile (400 mg) in THF was added sodium hydride (39 mg) and was stirred at 0-5° C. for less than five minutes. After completion, the reaction solvent was evaporated under vacuum and the crude solid obtained was quenched with ice water and subsequently neutralized by dilute HCl. The precipitate thus obtained was filtered and purified on a silica gel column using ethyl acetate-hexane as eluent. Yellow solid; mp 166-167° C.; ESIMS 415 (M++1); IR (KBr) 2218 (CN), 1712 cm−1 (CO); HRMS calcd. for C9H22N2O 414.1732. Found 414.1735.

後処理

  1. customAfter completion, the reaction solvent was evaporated under vacuum
  2. customthe crude solid obtained
  3. customwas quenched with ice water
  4. customThe precipitate thus obtained
  5. filtrationwas filtered
  6. custompurified on a silica gel column

出典と根拠

ORDレコード
ord-a738467d2f354b1c90aaa93cf17431e9
出典データセット
uspto-grants-2015_02
特許番号
US08946682B2

反応ノート

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