Ethanol → HCID 178517575、化合物

HRID 2278858ノート

反応式

HRID 2278858 の反応式
[CH:1]1([C:6](=O)[C:7]([O:9]CC)=O)[CH2:5][CH2:4][CH2:3][CH2:2]1.[F:13][C:14]1[CH:33]=[CH:32][CH:31]=[CH:30][C:15]=1[CH2:16][N:17]1[C:21]2=[N:22][CH:23]=N[CH:25]=[C:20]2[C:19]([C:26](=[NH:29])[NH:27][NH2:28])=[N:18]1.[CH2:34](O)C>>[CH:1]1([C:6]2[N:28]=[N:27][C:26]([C:19]3[C:20]4[C:21](=[N:22][CH:23]=[CH:34][CH:25]=4)[N:17]([CH2:16][C:15]4[CH:30]=[CH:31][CH:32]=[CH:33][C:14]=4[F:13])[N:18]=3)=[N:29][C:7]=2[OH:9])[CH2:2][CH2:3][CH2:4][CH2:5]1

参加物

4

反応物 3

HCID 702Ethanol2 回HCID 10953950Ethyl 2-cyclopentyl-2-oxoacetateHCID 178512736HCID 178512736、化合物

生成物 1

HCID 178517575HCID 178517575、化合物

実験手順

1.197 g (7.035 mmol) of ethyl cyclopentyl(oxo)acetate in 15 ml of ethanol were initially introduced and heated to reflux. Then, 2.000 g (7.035 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-d]pyrimidine-3-carboximidohydrazide suspended in 20 ml of ethanol were added and the mixture was heated under reflux overnight. After cooling, the mixture was concentrated and the residue was purified by preparative HPLC (mobile phase: acetonitrile/water with 0.1% TFA, ratio 45:55). This gave 749 mg of the target compound (26% of theory).

後処理

  1. temperatureheated to reflux
  2. additionwere added
  3. temperaturethe mixture was heated
  4. temperatureunder reflux overnight
  5. temperatureAfter cooling
  6. concentrationthe mixture was concentrated
  7. customthe residue was purified by preparative HPLC (mobile phase: acetonitrile/water with 0.1% TFA, ratio 45:55)

出典と根拠

ORDレコード
ord-3c2ebb481f5447a69ec8464f365e33b3
出典データセット
uspto-grants-2015_09
特許番号
US09133191B2

反応ノート

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