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HCID 67326745、化合物 → HCID 178510193、化合物

HRID 1500777
ノート
印刷プレビュー

反応式

HRID 1500777 の反応式
[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([OH:8])[CH2:4][CH2:3]1.[C:9]([C:11]1[CH:16]=[CH:15][N:14]2[N:17]=[CH:18][C:19]([C:20]3[N:25]=[C:24](N[C@@H]4CCCN(C(OC(C)(C)C)=O)C4)[CH:23]=[CH:22][N:21]=3)=[C:13]2[CH:12]=1)#[N:10]>CN(C=O)C>[OH:8][C@H:5]1[CH2:6][CH2:7][C@H:2]([NH:1][C:22]2[CH:23]=[CH:24][N:25]=[C:20]([C:19]3[CH:18]=[N:17][N:14]4[CH:15]=[CH:16][C:11]([C:9]#[N:10])=[CH:12][C:13]=34)[N:21]=2)[CH2:3][CH2:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 67326745HCID 67326745、化合物HCID 178511715HCID 178511715、化合物

生成物 1

HCID 178510193HCID 178510193、化合物収率 67%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Trans-4-aminocyclohexanol (85 mg, 0.74 mmol) was added to a solution of 3-(4-(1H-benzo[d][1,2,3]triazol-1-yloxy)pyrimidin-2-yl)pyrazolo[1,5-a]pyridine-5-carbonitrile (byproduct of Preparation 7a, 105 mg, 0.30 mmol) in N,N′-dimethylformamide (3 mL) and the mixture was stirred at ambient temperature overnight. The solvent was then evaporated and the residue was partitioned between water and ethyl acetate. The organic layer was separated, washed with water and brine, dried (MgSO4) and the solvent evaporated. The crude product was purified by flash chromatography (dichloromethane to 9:1 dichloromethane/methanol) to give the title compound (66 mg, 67%) as a yellow solid.

後処理

  1. customThe solvent was then evaporated
  2. customthe residue was partitioned between water and ethyl acetate
  3. customThe organic layer was separated
  4. washwashed with water and brine
  5. dry with materialdried (MgSO4)
  6. customthe solvent evaporated
  7. customThe crude product was purified by flash chromatography (dichloromethane to 9:1 dichloromethane/methanol)

出典と根拠

ORDレコード
ord-e23118c7a60e49f695e07740c09b3083
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09206183B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート