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Lithium Hydroxide → 4-[3-Butyl-3-(5,5,8,8-Tetramethyl-5,6,7,8-Tetrahydro-Naphthalen-2-yl)-Ureido]-Benzoic Acid

HRID 1760831
ノート
印刷プレビュー

反応式

HRID 1760831 の反応式
[CH2:1]([N:5]([C:20]1[CH:29]=[CH:28][C:27]2[C:26]([CH3:31])([CH3:30])[CH2:25][CH2:24][C:23]([CH3:33])([CH3:32])[C:22]=2[CH:21]=1)[C:6](=[O:19])[NH:7][C:8]1[CH:18]=[CH:17][C:11]([C:12]([O:14]CC)=[O:13])=[CH:10][CH:9]=1)[CH2:2][CH2:3][CH3:4].[OH-].[Li+]>CO.C1COCC1.O>[CH2:1]([N:5]([C:20]1[CH:29]=[CH:28][C:27]2[C:26]([CH3:31])([CH3:30])[CH2:25][CH2:24][C:23]([CH3:32])([CH3:33])[C:22]=2[CH:21]=1)[C:6](=[O:19])[NH:7][C:8]1[CH:18]=[CH:17][C:11]([C:12]([OH:14])=[O:13])=[CH:10][CH:9]=1)[CH2:2][CH2:3][CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 3939Lithium HydroxideHCID 22596834Ethyl 4-[3-butyl-3-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-ureido]-benzoate

生成物 1

HCID 225968404-[3-Butyl-3-(5,5,8,8-Tetramethyl-5,6,7,8-Tetrahydro-Naphthalen-2-yl)-Ureido]-Benzoic Acid収率 28%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

A solution of ethyl 4-[3-butyl-3-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-ureido]-benzoate (11) (131 mg, 0.29 mmole) in 15 mL methanol, 5 mL of THF and 5 mL of water was treated with 62 mg of lithium hydroxide (5 eq.) and stirred at room temperature for eight hours. The mixture was concentrated in vacuo and the residue was acidified with concentrated HCl solution. The mixture was then extracted with three portions of 20 mL of ethyl acetate. The combined organic extracts were dried over MgSO4, filtered and concentrated in vacuo to give a yellow solid which was purified by flash chromatography (SiO2, 20% ethyl acetate/hexanes+drops of acetic acid) to provide 34 mg (28%) of 4-[3-butyl-3-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-ureido]-benzoic acid (5) as a pale yellow solid. MS (EI): (M++1) 423.

後処理

  1. concentrationThe mixture was concentrated in vacuo
  2. extractionThe mixture was then extracted with three portions of 20 mL of ethyl acetate
  3. dry with materialThe combined organic extracts were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customto give a yellow solid which
  7. customwas purified by flash chromatography (SiO2, 20% ethyl acetate/hexanes+drops of acetic acid)

出典と根拠

ORDレコード
ord-a46c72cb9d474e0c87642493c4a73224
出典データセット
uspto-grants-2005_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06844466B2

反応ノート

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