Isopropylamine → HCID 70864655、化合物

HRID 2063256ノート

反応式

HRID 2063256 の反応式
[CH:1]([NH2:4])([CH3:3])[CH3:2].Cl[C:6]1[N:11]=[C:10]([C:12]2[C:13]([C:31]3[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=3)=[N:14][N:15]3[CH2:20][CH2:19][N:18]([C:21]([O:23][CH2:24][C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)=[O:22])[CH2:17][C:16]=23)[CH:9]=[CH:8][N:7]=1>>[F:37][C:34]1[CH:35]=[CH:36][C:31]([C:13]2[C:12]([C:10]3[CH:9]=[CH:8][N:7]=[C:6]([NH:4][CH:1]([CH3:3])[CH3:2])[N:11]=3)=[C:16]3[CH2:17][N:18]([C:21]([O:23][CH2:24][C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)=[O:22])[CH2:19][CH2:20][N:15]3[N:14]=2)=[CH:32][CH:33]=1

参加物

3

反応物 2

HCID 6363IsopropylamineHCID 86761634HCID 86761634、化合物2 回

生成物 1

HCID 70864655HCID 70864655、化合物

実験手順

A solution of isopropylamine (2.0 mL) and phenylmethyl 3-(2-chloro-4-pyrimidinyl)-2-(4-fluorophenyl)-6,7-dihydropyrazolo[1,5-a]pyrazine-5(4H)-carboxylate (i.e. the product of Step C) (1.00 g, 2.05 mmol) was heated in a sealed tube at 80° C. in a microwave reactor for 8 h. The reaction mixture was concentrated under reduced pressure to remove the excess amine. The residue was diluted with dichloromethane (50 mL) and treated with silica gel (10.0 g). The silica gel suspension was concentrated to leave a mixture of silica gel and crude product, which was purified by silica gel chromatography using a gradient of ethyl acetate/hexanes (0:1 to 7:1) as eluant to give 0.5 g of the title compound as a white solid.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customto remove the excess amine
  3. additionThe residue was diluted with dichloromethane (50 mL)
  4. additiontreated with silica gel (10.0 g)
  5. concentrationThe silica gel suspension was concentrated
  6. customto leave
  7. additiona mixture of silica gel and crude product, which
  8. customwas purified by silica gel chromatography

出典と根拠

ORDレコード
ord-d6f9b422c4f742d7b3ab2f08d85ed9ab
出典データセット
uspto-grants-2012_10
特許番号
US08288375B2

反応ノート

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