Sodium Hydroxide → 2-[1-[3'-(1-Methyl-3-pentylureido)biphenyl-4-yl]meth-(e)-ylidene]butyric acid

HRID 390611ノート

反応式

HRID 390611 の反応式
[OH-].[Na+].[CH3:3][N:4]([C:13]1[CH:14]=[C:15]([C:19]2[CH:24]=[CH:23][C:22](/[CH:25]=[C:26](\[CH2:32][CH3:33])/[C:27]([O:29]CC)=[O:28])=[CH:21][CH:20]=2)[CH:16]=[CH:17][CH:18]=1)[C:5]([NH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])=[O:6]>C(O)C.C(OCC)C>[CH3:3][N:4]([C:13]1[CH:14]=[C:15]([C:19]2[CH:24]=[CH:23][C:22](/[CH:25]=[C:26](\[CH2:32][CH3:33])/[C:27]([OH:29])=[O:28])=[CH:21][CH:20]=2)[CH:16]=[CH:17][CH:18]=1)[C:5]([NH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])=[O:6]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 68958868Ethyl 2-[1-[3'-(1-methyl-3-pentylureido)biphenyl-4-yl]meth-(e)-ylidene]butyrate

生成物 1

HCID 162244242-[1-[3'-(1-Methyl-3-pentylureido)biphenyl-4-yl]meth-(e)-ylidene]butyric acid収率 84%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒

反応条件

温度
50 °C

実験手順

268 mg (6.7 mmol) of sodium hydroxide are added to a solution of 284 mg (0.67 mmol) of ethyl 2-[1-[3′-(1-methyl-3-pentylureido)biphenyl-4-yl]meth-(E)-ylidene]butyrate in 10 mL of ethanol. The reaction mixture is heated at 50° C. for 15 hours. The reaction medium is evaporated to dryness, taken up in water, acidified with 2 N hydrochloric acid solution and extracted with ethyl acetate. The organic phases are combined, washed with water and dried over magnesium sulfate. After filtration, the solvent is evaporated off and the solid obtained is taken up in ethyl ether, filtered off and dried. 222 mg (84%) of 2-[1-[3′-(1-methyl-3-pentylureido)biphenyl-4-yl]meth-(E)-ylidene]butyric acid are obtained in the form of a white powder with a melting point of 150-152° C.

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. filtrationAfter filtration
  6. customthe solvent is evaporated off
  7. customthe solid obtained
  8. filtrationfiltered off
  9. customdried

出典と根拠

ORDレコード
ord-b76868267bfa4044a3186fc5f40b8959
出典データセット
uspto-grants-2013_02
特許番号
US08383652B2

反応ノート

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