3-Hydroxy-2,2-diphenylpropanenitrile → HCID 18626554、化合物

HRID 1685307ノート

反応式

HRID 1685307 の反応式
[OH:1][CH2:2][C:3]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[C:4]#[N:5].[H-].[H-].[H-].[H-].[Li+].[Al+3]>O1CCCC1>[NH2:5][CH2:4][C:3]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH2:2][OH:1]

参加物

4

反応物 2

HCID 202707253-Hydroxy-2,2-diphenylpropanenitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 18626554HCID 18626554、化合物収率 88%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 3-hydroxy-2,2-diphenylpropanenitrile in tetrahydrofuran (50 mL) was slowly added dropwise to a suspension of LAH in tetrahydrofuran (20 mL) at 23° C. The reaction was stirred overnight, then quenched with sodium sulfate decahydrate. The resulting solid was removed by filtration and the filtrate was concentrated to dryness to give the title material (0.45 g, 88%) as an oil which was used as such for the next reaction. 1H NMR (400 MHz, CDCl3) δ ppm: 2.49 (2H, s), 3.77 (1H, ddd, J=6.63, 4.23 and 2.53 Hz), 3.82 (2H, s), 4.30 (2H, s), 7.25-7.36 (10H, m). LC/MS (M+H)+: 228. HPLC ret. time (Condition A): 1.228 min.

後処理

  1. customquenched with sodium sulfate decahydrate
  2. customThe resulting solid was removed by filtration
  3. concentrationthe filtrate was concentrated to dryness

出典と根拠

ORDレコード
ord-9caa8114c2f0461f936be1f2ba086ac4
出典データセット
uspto-grants-2012_04
特許番号
US08148400B2

反応ノート

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