Sodium Hydroxide → 5-Propylcarbamoyl-biphenyl-3-carboxylic acid

HRID 2421620ノート

反応式

HRID 2421620 の反応式
[OH-].[Na+].C[O:4][C:5]([C:7]1[CH:8]=[C:9]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:10]=[C:11]([C:13](=[O:18])[NH:14][CH2:15][CH2:16][CH3:17])[CH:12]=1)=[O:6]>CO.CC(C)=O.O.Cl>[CH2:15]([NH:14][C:13]([C:11]1[CH:12]=[C:7]([C:5]([OH:6])=[O:4])[CH:8]=[C:9]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:10]=1)=[O:18])[CH2:16][CH3:17]

参加物

7

反応物 2

HCID 14798Sodium Hydroxide2 回HCID 67214482HCID 67214482、化合物

生成物 1

HCID 672136885-Propylcarbamoyl-biphenyl-3-carboxylic acid

試薬・触媒・溶媒 4

HCID 313Hydrochloric Acid触媒HCID 180Acetone溶媒HCID 887Methanol溶媒2 回HCID 962Water溶媒

実験手順

A solution of NaOH (44 mg, 1.1 mmol) in 372 μL of MeOH was added to a solution of 68D (284 mg, 0.96 mmol) in 1.8 mL of acetone. The reaction was stirred at room temperature for 16 hrs after which time 10 mg of NaOH and 200 μL of MeOH were added. The reaction was stirred for 72 hrs. The reaction mixture was then concentrated in vacuo and the residue obtained was dissolved in water and a few drops of concentrated HCl were added till pH ˜1. An off-white solid appeared. It was collected by filtration and extensively rinsed with water. The solid was then dried in vacuo (194 mg, 72%). NMR 1H (ppm, CD3OD): 8.43 (t., J4=1.63 Hz, 1H), 8.38 (t., J4=1.73 Hz, 1H), 8.27 (t., J4=1.78 Hz, 1H), 7.71-7.67 (m, 2H), 7.48 (m, 2H), 7.39 (t.t., J3=7.34 Hz, J4=1.36 Hz 1H), 3.39-3.34 (m, 2H), 1.65 (sext., J3=7.18 Hz, 2H), 0.98 (t., J3=7.34 Hz, 3H).

後処理

  1. additionwere added
  2. concentrationThe reaction mixture was then concentrated in vacuo
  3. customthe residue obtained
  4. filtrationIt was collected by filtration
  5. washextensively rinsed with water
  6. customThe solid was then dried in vacuo (194 mg, 72%)

出典と根拠

ORDレコード
ord-4ac2da28136a482f8a83934926045470
出典データセット
uspto-grants-2011_06
特許番号
US07956216B2

反応ノート

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