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Cyclopropanecarbonyl chloride → N'-(Cyclopropylcarbonyl)-1-ethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridine-5-carbohydrazide

HRID 490886
ノート
印刷プレビュー

反応式

HRID 490886 の反応式
Cl.Cl.[CH2:3]([N:5]1[C:9]2=[N:10][CH:11]=[C:12]([C:21]([NH:23][NH2:24])=[O:22])[C:13]([NH:14][CH:15]3[CH2:20][CH2:19][O:18][CH2:17][CH2:16]3)=[C:8]2[CH:7]=[N:6]1)[CH3:4].CCN(C(C)C)C(C)C.[CH:34]1([C:37](Cl)=[O:38])[CH2:36][CH2:35]1>C1COCC1>[CH:34]1([C:37]([NH:24][NH:23][C:21]([C:12]2[C:13]([NH:14][CH:15]3[CH2:16][CH2:17][O:18][CH2:19][CH2:20]3)=[C:8]3[CH:7]=[N:6][N:5]([CH2:3][CH3:4])[C:9]3=[N:10][CH:11]=2)=[O:22])=[O:38])[CH2:36][CH2:35]1
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 77637Cyclopropanecarbonyl chlorideHCID 81531DiisopropylethylamineHCID 534878281-Ethyl-4-((tetrahydro-2H-pyran-4-yl)amino)-1H-pyrazolo[3,4-b]pyridine-5-carbohydrazide dihydrochloride

生成物 1

HCID 57675148N'-(Cyclopropylcarbonyl)-1-ethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridine-5-carbohydrazide収率 45%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

A solution of Intermediate 19 (0.045 g) in THF (2 ml) was treated with DIPEA (0.045 ml), then with cyclopropylcarbonyl chloride (0.013 g) and stirred at room temperature for 16 h. The mixture was concentrated in vacuo and the residue partitioned between dichloromethane and water. The layers were separated and the organic layer concentrated in vacuo, then applied to an SPE cartridge (aminopropyl, 1 g). The column was eluted with methanol to afford Intermediate 20 as a white solid (0.02 g). LCMS showed MH+=373; TRET=2.15 min.

後処理

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue partitioned between dichloromethane and water
  3. customThe layers were separated
  4. concentrationthe organic layer concentrated in vacuo
  5. washThe column was eluted with methanol

出典と根拠

ORDレコード
ord-5644c95b75ba4d8da6d565b0e8131feb
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07528148B2

反応ノート

読み込み中…

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