Lithium hydroxide, monohydrate → (e)-[4-[3-(4-Chlorophenyl)-3-[4-[3-(4-methylpiperazin-1-yl)propynyl]phenyl]allyloxy]-2-methylphenoxy]acetic acid

HRID 1810674ノート

反応式

HRID 1810674 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5](/[C:8](/[C:25]2[CH:30]=[CH:29][C:28]([C:31]#[C:32][CH2:33][N:34]3[CH2:39][CH2:38][N:37]([CH3:40])[CH2:36][CH2:35]3)=[CH:27][CH:26]=2)=[CH:9]/[CH2:10][O:11][C:12]2[CH:23]=[CH:22][C:15]([O:16][CH2:17][C:18]([O:20]C)=[O:19])=[C:14]([CH3:24])[CH:13]=2)=[CH:4][CH:3]=1.O.[OH-].[Li+]>C(O)C.O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5](/[C:8](/[C:25]2[CH:30]=[CH:29][C:28]([C:31]#[C:32][CH2:33][N:34]3[CH2:35][CH2:36][N:37]([CH3:40])[CH2:38][CH2:39]3)=[CH:27][CH:26]=2)=[CH:9]/[CH2:10][O:11][C:12]2[CH:23]=[CH:22][C:15]([O:16][CH2:17][C:18]([OH:20])=[O:19])=[C:14]([CH3:24])[CH:13]=2)=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 86629309methyl (E)-[4-[3-(4-chlorophenyl)-3-[4-[3-(4-methylpiperazin-1-yl)propynyl]phenyl]-allyloxy]-2-methyl-phenoxy]acetate

生成物 1

HCID 23633562(e)-[4-[3-(4-Chlorophenyl)-3-[4-[3-(4-methylpiperazin-1-yl)propynyl]phenyl]allyloxy]-2-methylphenoxy]acetic acid

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

The above ester (0.36 g, 0.658 mmol) was dissolved in ethanol (30 mL), a solution of lithium hydroxide monohydrate (0.10 g, 2.38 mmol) in water (4 mL) was added and the mixture was left to stand for 72 h. The solvents were evaporated in vacuo; the residue was diluted with water (25 mL), acidified with acetic acid (0.25 mL) and extracted with chloroform (2×50 mL). The organic solution was dried with anhydrous potassium carbonate and subsequently evaporated in vacuo. The residue was triturated with hexanes (2×20 mL) yielding the title compound as amorphous solid.

後処理

  1. waitthe mixture was left
  2. customThe solvents were evaporated in vacuo
  3. additionthe residue was diluted with water (25 mL)
  4. extractionextracted with chloroform (2×50 mL)
  5. dry with materialThe organic solution was dried with anhydrous potassium carbonate
  6. customsubsequently evaporated in vacuo
  7. customThe residue was triturated with hexanes (2×20 mL)

出典と根拠

ORDレコード
ord-32ac71c5e2d846ecad45f8aceb34ce21
出典データセット
uspto-grants-2013_01
特許番号
US08362016B2

反応ノート

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