Dimethylamine → HCID 178473725, 화합물

HRID 849427노트

반응식

HRID 849427 반응식
[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]

참가 물질

4

반응물 2

HCID 674DimethylamineHCID 178478619HCID 178478619, 화합물

생성물 1

HCID 178473725HCID 178473725, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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

후처리

  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)

출처 및 근거

ORD 기록
ord-bef3c84f2173493c8b17d8738e0126f7
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06011029

반응 노트

불러오는 중…