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Acetone → 2-(2,3-Dimethyl-4-(2-methyl-4-nitro-1H-indol-5-yloxy)phenyl)acetic acid

HRID 2423288
ノート
印刷プレビュー

反応式

HRID 2423288 の反応式
[NH2:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:12]=[CH:11][C:10]([CH2:13][C:14]([OH:16])=[O:15])=[C:9]([CH3:17])[C:8]=2[CH3:18])=[C:4]([N+:21]([O-:23])=[O:22])[CH:3]=1.[CH3:24][C:25]([CH3:27])=O.CC(C)([O-])C.[K+]>CS(C)=O.O.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>[CH3:17][C:9]1[C:8]([CH3:18])=[C:7]([O:6][C:5]2[C:4]([N+:21]([O-:23])=[O:22])=[C:3]3[C:2](=[CH:20][CH:19]=2)[NH:1][C:25]([CH3:27])=[CH:24]3)[CH:12]=[CH:11][C:10]=1[CH2:13][C:14]([OH:16])=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 180AcetoneHCID 23665647Potassium tert-butoxideHCID 598648252-(4-(4-Amino-2-nitrophenoxy)-2,3-dimethylphenyl)acetic acid

生成物 1

HCID 598648942-(2,3-Dimethyl-4-(2-methyl-4-nitro-1H-indol-5-yloxy)phenyl)acetic acid

試薬・触媒・溶媒 3

HCID 311Citric Acid溶媒
HCID 679
Dimethyl Sulfoxide
溶媒
HCID 962Water溶媒

実験手順

Under an N2 atmosphere, 2-(4-(4-amino-2-nitrophenoxy)-2,3-dimethylphenyl)acetic acid (0.723 g, 2.29 mmol) was dissolved in DMSO (18 mL) and acetone (0.503 mL, 6.86 mmol) was added. The reaction was treated with potassium tert-butoxide (0.770 g, 6.86 mmol) and allowed to stir at room temperature for 1.5 h. The reaction was diluted with water and citric acid was added to pH 4. The mixture was extracted with ethyl acetate. The aqueous layer was washed with additional ethyl acetate. The organics were combined, dried (Na2SO4), filtered and concentrated in vacuo. Flash column chromatography of the residue, eluting with 0% to 9% methanol in dichloromethane, afforded the title compound. LC-MS ESI (neg.) m/z: 353.2 (M−H).

後処理

  1. additionwas added to pH 4
  2. extractionThe mixture was extracted with ethyl acetate
  3. washThe aqueous layer was washed with additional ethyl acetate
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. washFlash column chromatography of the residue, eluting with 0% to 9% methanol in dichloromethane

出典と根拠

ORDレコード
ord-536bbeed8fda4a5985f59be436375e90
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07960567B2

反応ノート

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