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Potassium Carbonate → HCID 68508572、化合物

HRID 1947080
ノート
印刷プレビュー

反応式

HRID 1947080 の反応式
[Cl:1][C:2]1[C:3]([C:8]([F:11])([F:10])[F:9])=[N:4][NH:5][C:6]=1[CH3:7].C(=O)([O-])[O-].[K+].[K+].[C:18]([O:22][C:23](=[O:26])CBr)([CH3:21])([CH3:20])[CH3:19]>C(#N)C>[C:18]([O:22][C:23]([N:5]1[C:6]([CH3:7])=[C:2]([Cl:1])[C:3]([C:8]([F:9])([F:11])[F:10])=[N:4]1)=[O:26])([CH3:21])([CH3:20])[CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 79177tert-Butyl bromoacetateHCID 12069654-Chloro-5-methyl-3-(trifluoromethyl)-1H-pyrazole

生成物 1

HCID 68508572HCID 68508572、化合物収率 95%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To 2.70 mmol of 4-chloro-5-methyl-3-trifluoromethylpyrazole and 3.9 mmol of potassium carbonate in 0.5M solution of acetonitrile add 3.25 mmol of t-butylbromoacetate. The reaction was allowed to stir at room temperature for an hour and then heated at 70° C. for 12 hours. The reaction was filtered, the filtrate concentrated to a crude oil. Fresh ether was added and the mixture was allowed to cool. The white crystals obtained were filtered and vaccum dried to give the desired intermediate 4-chloro-5-methyl -3-trifluoromethyl pyrazole-1-carboxylic acid tertbutyl ester in 95% yield. LC-MS in FP m/z=300 (M++1)

後処理

  1. temperatureheated at 70° C. for 12 hours
  2. filtrationThe reaction was filtered
  3. concentrationthe filtrate concentrated to a crude oil
  4. additionFresh ether was added
  5. temperatureto cool
  6. customThe white crystals obtained
  7. filtrationwere filtered
  8. customvaccum dried

出典と根拠

ORDレコード
ord-d74d2f99165b443a8d8f9f2631d8231d
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399455B2

反応ノート

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