Propionyl chloride → HCID 57717542、化合物

HRID 1360538ノート

反応式

HRID 1360538 の反応式
[NH2:1][C:2]([CH3:22])([CH3:21])[CH2:3][C:4]1[N:5]([CH2:18][CH2:19][CH3:20])[N:6]=[C:7]2[C:16]=1[C:15]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N:9]=[C:8]2[NH2:17].[C:23](Cl)(=[O:26])[CH2:24][CH3:25]>>[NH2:17][C:8]1[C:7]2=[N:6][N:5]([CH2:18][CH2:19][CH3:20])[C:4]([CH2:3][C:2]([NH:1][C:23](=[O:26])[CH2:24][CH3:25])([CH3:21])[CH3:22])=[C:16]2[C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[N:9]=1

参加物

3

反応物 2

HCID 62324Propionyl chlorideHCID 57717565HCID 57717565、化合物

生成物 1

HCID 57717542HCID 57717542、化合物収率 77.1%

実験手順

Using the method of Example 68, 1-(2-amino-2-methylpropyl)-2-propyl-2H-pyrazolo[3,4-c]quinolin-4-amine (prepared as described in Example 64, 595 mg, 2.00 mmol) was reacted with propionyl chloride (463 mg, 5.00 mmol). The crude product was purified by IFC (silica gel eluting with a gradient of 15 to 25% CMA in chloroform) followed by recrystallization from ethyl acetate/hexanes to provide 545 mg of N-[2-(4-amino-2-propyl-2H-pyrazolo[3,4-c]quinolin-1-yl)-1,1-dimethylethyl]propionamide as a white solid, mp 158-159° C. MS (APCI) m/z 354 (M+H)+; Anal. Calcd for C20H27N5O: C, 67.96; H, 7.70; N, 19.81. Found: C, 67.80; H, 8.08; N, 19.77

後処理

  1. customThe crude product was purified by IFC (silica gel eluting with a gradient of 15 to 25% CMA in chloroform)
  2. customfollowed by recrystallization from ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-dea1e9031c2b406e9bddabf7a98f6345
出典データセット
uspto-grants-2011_02
特許番号
US07879849B2

反応ノート

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