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Water → 1-((2-Fluorophenyl)methyl)pyrazolo(3,4-b)pyridine-3-carbonitrile

HRID 346528
ノート
印刷プレビュー

反応式

HRID 346528 の反応式
[F:1][C:2]1[CH:20]=[CH:19][CH:18]=[CH:17][C:3]=1[CH2:4][N:5]1[C:9]2=[N:10][CH:11]=[CH:12][CH:13]=[C:8]2[C:7]([C:14]([NH2:16])=O)=[N:6]1.N1C=CC=CC=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.O>C1COCC1>[C:14]([C:7]1[C:8]2[C:9](=[N:10][CH:11]=[CH:12][CH:13]=2)[N:5]([CH2:4][C:3]2[CH:17]=[CH:18][CH:19]=[CH:20][C:2]=2[F:1])[N:6]=1)#[N:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 9845Trifluoroacetic anhydrideHCID 113231781-(2-Fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboxamide

生成物 1

HCID 114025001-((2-Fluorophenyl)methyl)pyrazolo(3,4-b)pyridine-3-carbonitrile

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒

実験手順

36.1 g (133 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboxamide from Example 3A are dissolved in 330 ml of THF, and 27 g (341 mmol) of pyridine are added. Then, over the course of 10 minutes, 47.76 ml (71.66 g, 341 mmol) of trifluoroacetic anhydride are added, during which the temperature rises to 40° C. The mixture is stirred at room temperature overnight. It is then added to 1 l of water and extracted three times with 0.5 l of ethyl acetate each time. The organic phase is washed with saturated sodium bicarbonate solution and with 1N hydrochloric acid, dried with magnesium sulphate and concentrated in a rotary evaporator.

後処理

  1. customrises to 40° C
  2. extractionextracted three times with 0.5 l of ethyl acetate each time
  3. washThe organic phase is washed with saturated sodium bicarbonate solution and with 1N hydrochloric acid
  4. dry with materialdried with magnesium sulphate
  5. concentrationconcentrated in a rotary evaporator

出典と根拠

ORDレコード
ord-aa7c50844f5a4f9eb27ac5a42c48c6cf
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07173037B2

反応ノート

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