Ethanol → HCID 178517575, 화합물

HRID 2278858노트

반응식

HRID 2278858 반응식
[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

참가 물질

4

반응물 3

HCID 702Ethanol2회HCID 10953950Ethyl 2-cyclopentyl-2-oxoacetateHCID 178512736HCID 178512736, 화합물

생성물 1

HCID 178517575HCID 178517575, 화합물

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-3c2ebb481f5447a69ec8464f365e33b3
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133191B2

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