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Hydrochloric Acid → [5-(4-Hydroxy-2-methyl-phenyl)-1H-indol-3-yl]-acetic acid methyl ester

HRID 250235
ノート
印刷プレビュー

反応式

HRID 250235 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([OH:17])[CH:5]=[CH:6][C:7]=1B1OC(C)(C)C(C)(C)O1.[CH3:18][O:19][C:20](=[O:32])[CH2:21][C:22]1[C:30]2[C:25](=[CH:26][CH:27]=[C:28](Br)[CH:29]=2)[NH:24][CH:23]=1.C(=O)([O-])[O-].[K+].[K+].Cl>O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C(O)C.CN(C=O)C>[CH3:18][O:19][C:20](=[O:32])[CH2:21][C:22]1[C:30]2[C:25](=[CH:26][CH:27]=[C:28]([C:7]3[CH:6]=[CH:5][C:4]([OH:17])=[CH:3][C:2]=3[CH3:1])[CH:29]=2)[NH:24][CH:23]=1
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

9

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 49782545methyl 2-(5-bromo-1H-indol-3-yl)acetateHCID 574432723-Methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenol

生成物 1

HCID 57443276[5-(4-Hydroxy-2-methyl-phenyl)-1H-indol-3-yl]-acetic acid methyl ester収率 60%

試薬・触媒・溶媒 4

HCID 178418397
HCID 178418397、化合物
触媒
HCID 702Ethanol溶媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

A mixture of 3-methyl-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenol (287 mg, 1.22 mmol), (5-bromo-1H-indol-3-yl)-acetic acid methyl ester (273 mg, 1.02 mmol), tetrakis(triphenylphosphine)palladium(0) (57 mg, 0.046 mmol), DMF (2.7 mL), ethanol (1.34 mL) and 2M aqueous potassium carbonate (1.34 mL) is heated to 100° C. for 16 hours. The reaction is cooled to room temperature and diluted with water and acidified with 1 N HCl. The resulting solution is extracted with ethyl acetate. The combined organic layers are dried over anhydrous magnesium sulfate and concentrated. The residue is dissolved in methanol (6 mL) and trimethylsilyldiazomethane (2.0 M solution in hexanes, approximately 4 mL) is added over approximately two minutes at room temperature. The yellow mixture is concentrated and the residue is purified via radial chromatography eluting with a gradient of 20 to 50% ethyl acetate/heptane and crystallized from CH2Cl2/heptane to give the title compound (180 mg, 60%). ES/MS m/e 296.1 (M+1).

後処理

  1. temperatureThe reaction is cooled to room temperature
  2. extractionThe resulting solution is extracted with ethyl acetate
  3. dry with materialThe combined organic layers are dried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. dissolutionThe residue is dissolved in methanol (6 mL)
  6. additiontrimethylsilyldiazomethane (2.0 M solution in hexanes, approximately 4 mL) is added over approximately two minutes at room temperature
  7. concentrationThe yellow mixture is concentrated
  8. customthe residue is purified via radial chromatography
  9. washeluting with a gradient of 20 to 50% ethyl acetate/heptane
  10. customcrystallized from CH2Cl2/heptane

出典と根拠

ORDレコード
ord-6c748b5b1e674c0b862ae067754ee53b
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07863302B2

反応ノート

読み込み中…

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