Hydrochloric Acid → HCID 68536680、化合物

HRID 969723

反応式

HRID 969723 の反応式
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8]([S:15]([N:18]=[CH:19][N:20]([CH3:22])[CH3:21])(=[O:17])=[O:16])=[C:9]([C:11]([F:14])([F:13])[F:12])[N:10]=2)[N:7]=1.[Br-].[CH2:24]([Zn+])[CH2:25][CH3:26].O.Cl>O1CCCC1.Cl[Ni]1(Cl)[P](C2C=CC=CC=2)(C2C=CC=CC=2)CCC[P]1(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:21][N:20]([CH3:22])[CH:19]=[N:18][S:15]([C:8]1[N:6]2[N:7]=[C:2]([CH2:24][CH2:25][CH3:26])[CH:3]=[CH:4][C:5]2=[N:10][C:9]=1[C:11]([F:14])([F:13])[F:12])(=[O:17])=[O:16]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 74015820HCID 74015820、化合物HCID 178455869HCID 178455869、化合物

生成物 1

HCID 68536680HCID 68536680、化合物

試薬・触媒・溶媒 2

HCID 178418745HCID 178418745、化合物触媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of N′-(6-chloro-2-trifluoromethylimidazo[1,2-b]pyridazin-3-ylsulfonyl)-N,N-dimethylformamidine (1.00 g, 2.81 mmol) and [1,3-bis(diphenylphosphino)propane]nickel(II) dichloride (0.076 g, 0.14 mmol) in tetrahydrofuran (8.0 ml) was added dropwise a solution of n-propylzinc bromide in tetrahydrofuran (0.5 M, 8.43 ml, 4.22 mmol) with stirring under ice-cooling and nitrogen stream. The reaction mixture was stirred for 30 minutes under ice-cooling and 4.5 hours at room temperature, then poured into cold water and made acid with dilute hydrochloric acid. The precipitated solid was collected by filtration, washed with dilute hydrochloric acid, then water, and purified by silica gel column chromatography (ethyl acetate:chloroform=2:5) to give the title compound as white crystals. The yield was 0.62 g (60.7%).

後処理

  1. temperaturecooling
  2. stirringThe reaction mixture was stirred for 30 minutes under ice-
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with dilute hydrochloric acid
  5. customwater, and purified by silica gel column chromatography (ethyl acetate:chloroform=2:5)

出典と根拠

ORDレコード
ord-47dc2caa5c5a40d288b9c1333f8cb7cf
出典データセット
uspto-grants-2007_12
特許番号
US07307165B2

関連ノート

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