Dimethylamine → HCID 178473725、化合物

HRID 849427ノート

反応式

HRID 849427 の反応式
[ClH:1].Cl.Cl.[NH:4]1[CH:8]=[C:7]([CH2:9][N:10]2[C:16]3[CH:17]=[CH:18][C:19]([C:21]4[CH:22]=N[CH:24]=[CH:25][CH:26]=4)=[CH:20][C:15]=3[CH2:14][N:13]([C:27](=[O:32])[C:28](F)(F)F)[CH:12]([CH2:33][C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[CH2:11]2)[N:6]=[CH:5]1.[CH3:40]NC>CN(C=O)C>[ClH:1].[C:27]([N:13]1[CH2:14][C:15]2[CH:20]=[C:19]([C:21]3[CH:22]=[CH:40][CH:24]=[CH:25][CH:26]=3)[CH:18]=[CH:17][C:16]=2[N:10]([CH2:9][C:7]2[N:6]=[CH:5][NH:4][CH:8]=2)[CH2:11][C@H:12]1[CH2:33][C:34]1[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=1)(=[O:32])[CH3:28]

参加物

4

反応物 2

HCID 674DimethylamineHCID 178478619HCID 178478619、化合物

生成物 1

HCID 178473725HCID 178473725、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of Compound B (7 g) and dimethylamine (2.0 M in THF, 75 mL, 150 mmol) in DMF (150 mL) was warmed to 80° C. (sealed tube) for 30 hr. The DMF was removed. The residue was passed through a short silica gel colum (5% MeOH, 0.5% NH4OH in CH2Cl2). The eluant was evaporated and the residue was purified by reverse phase preparative HPLC (gradient of aqueous methanol with 0.1% TFA) and converted to the HCl salt to provide Compound C as an off white solid (5.0 g, 60% from Compound D of Example 226) MS: (M+H)+ 544

後処理

  1. custom(sealed tube) for 30 hr
  2. customThe DMF was removed
  3. customThe eluant was evaporated
  4. customthe residue was purified by reverse phase preparative HPLC (gradient of aqueous methanol with 0.1% TFA)

出典と根拠

ORDレコード
ord-bef3c84f2173493c8b17d8738e0126f7
出典データセット
uspto-grants-2000_01
特許番号
US06011029

反応ノート

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