Tetrahydrofuran → HCID 58409925、化合物

HRID 1844906ノート

反応式

HRID 1844906 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[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH2:16][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]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:16](=[O:37])[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 58409919HCID 58409919、化合物

生成物 1

HCID 58409925HCID 58409925、化合物

反応条件

温度
2.5 °C

実験手順

A solution of 4-(naphthalen-2-yl)-2-(piperidin-1-yl)-9H-fluorene-1-carbonitrile (400 mg) in THF was added sodium hydride (32 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. Light red solid; mp 182-184° C.; ESIMS 415 (M++1); IR (KBr) 2213 (CN), 1695 cm−1 (CO).

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. additionby dilute HCL
  5. customThe precipitate thus obtained
  6. filtrationwas filtered
  7. custompurified on a silica gel column

出典と根拠

ORDレコード
ord-59d70f2d729249828aaa3d2308484666
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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