ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Sodium Hydroxide → 3-[3'-(3-Heptyl-1-methylureido)-2-(3-methylbutoxy)biphenyl-4-yl]propanoic acid

HRID 250850
ノート
印刷プレビュー

反応式

HRID 250850 の反応式
[OH-].[Na+].[CH2:3]([NH:10][C:11](=[O:38])[N:12]([C:14]1[CH:15]=[C:16]([C:20]2[CH:25]=[CH:24][C:23]([CH2:26][CH2:27][C:28]([O:30]C)=[O:29])=[CH:22][C:21]=2[O:32][CH2:33][CH2:34][CH:35]([CH3:37])[CH3:36])[CH:17]=[CH:18][CH:19]=1)[CH3:13])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9]>CO>[CH2:3]([NH:10][C:11](=[O:38])[N:12]([C:14]1[CH:15]=[C:16]([C:20]2[CH:25]=[CH:24][C:23]([CH2:26][CH2:27][C:28]([OH:30])=[O:29])=[CH:22][C:21]=2[O:32][CH2:33][CH2:34][CH:35]([CH3:37])[CH3:36])[CH:17]=[CH:18][CH:19]=1)[CH3:13])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 67271485Methyl 3-[3'-(3-heptyl-1-methylureido)-2-(3-methylbutoxy)biphenyl-4-yl]propanoate

生成物 1

HCID 115331433-[3'-(3-Heptyl-1-methylureido)-2-(3-methylbutoxy)biphenyl-4-yl]propanoic acid収率 84%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
55 °C

実験手順

281 mg (7.03 mmol, 10 eq) of sodium hydroxide are added to a solution of 400 mg (0.703 mmol, 1 eq) of methyl 3-[3′-(3-heptyl-1-methylureido)-2-(3-methylbutoxy)biphenyl-4-yl]propanoate in 10 ml of methanol. The reaction mixture is heated at 55° C. for 1 hour. The reaction medium is evaporated to dryness, taken up in water, acidified with 2N hydrochloric acid solution and extracted with ethyl acetate. The organic phases are combined, washed with water and dried over magnesium sulfate. The solvent is evaporated off and the oil obtained is chromatographed on silica gel (10 g FlashSmart column) eluted with 30/70 heptane/ethyl acetate. The product is crystallized from heptane and 284 mg of 3-[3′-(3-heptyl-1-methylureido)-2-(3-methylbutoxy)biphenyl-4-yl]propanoic acid are obtained in the form of white crystals (m.p.=60-62° C.). Yield=84%

後処理

  1. customThe reaction medium is evaporated to dryness
  2. extractionextracted with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent is evaporated off
  6. customthe oil obtained
  7. customis chromatographed on silica gel (10 g FlashSmart column)
  8. washeluted with 30/70 heptane/ethyl acetate
  9. customThe product is crystallized from heptane and 284 mg of 3-[3′-(3-heptyl-1-methylureido)-2-(3-methylbutoxy)biphenyl-4-yl]propanoic acid

出典と根拠

ORDレコード
ord-9549783122c84723bf1dcba770ee9c62
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07863332B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート