Sodium hydride → HCID 58409942、化合物

HRID 1844877ノート

反応式

HRID 1844877 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]1O[C:15](=O)[C:14]([C:18]#[N:19])=[C:13]([N:20]2[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]2)[CH:12]=1.[H-].[Na+]>C1COCC1>[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:12]2[CH2:11][C:2]3[C:1](=[CH:10][CH:5]=[CH:4][CH:3]=3)[C:15]=2[C:14]([C:18]#[N:19])=[C:13]([N:20]2[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]2)[CH:12]=1

参加物

4

反応物 2

HCID 24758Sodium hydrideHCID 110888242H-Pyran-3-carbonitrile, 6-(2-naphthalenyl)-2-oxo-4-(1-piperidinyl)-

生成物 1

HCID 58409942HCID 58409942、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 6-(naphthalen-2-yl)-2-oxo-4-(piperidin-1-yl)-2H-pyran-3-carbonitrile (330 mg), indanone-1 (132 mg) and NaH (39 mg) in THF was stirred for <5 min. After completion, the reaction solvent was evaporated under vacuum to dryness and crude, solid was quenched with ice water and subsequently neutralized with dil. HCl, finally purified by column chromatography using ethylacetate-hexane as eluent. White solid; mp 136-138° C.; ESIMS 401 (M++1); IR (KBr) 2214 cm−1 (CN); HRMS calcd. for C2H24N2 400.1940 Found 400.1939.

後処理

  1. customAfter completion, the reaction solvent was evaporated under vacuum to dryness and crude, solid
  2. customwas quenched with ice water
  3. customfinally purified by column chromatography

出典と根拠

ORDレコード
ord-09ab6418a39d4d54b008c011ecc69b57
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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