Lithium hydroxide, monohydrate → (E)-3-(3'-Adamantan-1-yl-4'-cyanomethoxybiphenyl-4-yl)-acrylic acid

HRID 41728ノート

反応式

HRID 41728 の反応式
C[O:2][C:3](=[O:32])/[CH:4]=[CH:5]/[C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:17]=[CH:16][C:15]([O:18][CH2:19][C:20]#[N:21])=[C:14]([C:22]34[CH2:31][CH:26]5[CH2:27][CH:28]([CH2:30][CH:24]([CH2:25]5)[CH2:23]3)[CH2:29]4)[CH:13]=2)=[CH:8][CH:7]=1.O[Li].O>C1COCC1.O>[C:22]12([C:14]3[CH:13]=[C:12]([C:9]4[CH:8]=[CH:7][C:6](/[CH:5]=[CH:4]/[C:3]([OH:32])=[O:2])=[CH:11][CH:10]=4)[CH:17]=[CH:16][C:15]=3[O:18][CH2:19][C:20]#[N:21])[CH2:23][CH:24]3[CH2:25][CH:26]([CH2:27][CH:28]([CH2:30]3)[CH2:29]1)[CH2:31]2

参加物

4

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 67399554(E)-3-(3'-adamantan-1-yl-4'-cyanomethoxybiphenyl-4-yl)-acrylic acid methyl ester

生成物 1

HCID 46830625(E)-3-(3'-Adamantan-1-yl-4'-cyanomethoxybiphenyl-4-yl)-acrylic acid

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

(E)-3-(3′-Adamantan-1-yl-4′-cyanomethoxybiphenyl-4-yl)-acrylic acid methyl ester (240 mg, 0.56 mmol) was added to a solution of LiOH.H2O (117 mg, 2.8 mmol) in 24 ml of THF:H2O 1:1. The solution thus obtained was kept under stirring at RT overnight. THF was removed under reduced pressure and the resulting aqueous layer acidified with 1N HCl to allow the formation of the title compound as a white precipitate that was filtered (216 mg, 93%).

後処理

  1. customThe solution thus obtained
  2. customTHF was removed under reduced pressure
  3. filtrationwas filtered (216 mg, 93%)

出典と根拠

ORDレコード
ord-bb5cc6a1eb00479a8f1f3673fb64a002
出典データセット
uspto-grants-2013_09
特許番号
US08530517B2

反応ノート

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