Hydrochloric Acid → 3-(3-Methylindan-1-ylidene)-1,3-dihydroindol-2-one

HRID 478705

反応式

HRID 478705 の反応式
[CH3:1][CH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=O)[CH2:3]1.[NH:12]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:14][C:13]1=[O:21].N1CCCCC1.Cl>CN(C)C=O>[CH3:1][CH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[C:14]2[C:15]3[C:20](=[CH:19][CH:18]=[CH:17][CH:16]=3)[NH:12][C:13]2=[O:21])[CH2:3]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8082PiperidineHCID 2595603-Methyl-indan-1-oneHCID 321710Oxindole

生成物 1

HCID 570344053-(3-Methylindan-1-ylidene)-1,3-dihydroindol-2-one収率 13.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
130 °C

実験手順

A mixture of 0.5 g of 3-methyl-1-indanone, 1.37 g oxindole and 5 ml piperidine in 3 ml of dimethylforamide was heated in a sealed tube at 130° C. overnight to yield a reddish-brown suspension. The mixture was added to 1N hydrochloric acid solution and extracted with ethyl acetate. The organic layer was washed with brine, dried with magnesium sulfate and concentrated. Chromatography afforded 120 mg of 3-(3-methylindan-1-ylidene)-1,3-dihydroindol-2-one as an orange solid.

後処理

  1. customto yield a reddish-brown suspension
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-93565151183748cd92aef058f334cf1e
出典データセット
uspto-grants-2003_11
特許番号
US06642251B1

関連ノート

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