1,1'-Carbonyldiimidazole → HCID 59394510、化合物

HRID 45115

反応式

HRID 45115 の反応式
[CH2:1]([O:8][CH2:9][C:10]1[N:15]=[CH:14][N:13]=[C:12]([O:16][C:17]2[CH:18]=[C:19]3[C:23](=[CH:24][CH:25]=2)[NH:22][CH:21]=[CH:20]3)[CH:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1N=CN([C:31]([N:33]2C=N[CH:35]=[CH:34]2)=[O:32])C=1.[CH3:38][O:39][C:40]1[CH:46]=CC(N)=[CH:42][C:41]=1[C:47]([F:50])([F:49])[F:48]>ClCCCl.C(Cl)Cl>[CH2:1]([O:8][CH2:9][C:10]1[N:15]=[CH:14][N:13]=[C:12]([O:16][C:17]2[CH:18]=[C:19]3[C:23](=[CH:24][CH:25]=2)[N:22]([C:31]([NH:33][C:34]2[CH:35]=[CH:46][C:40]([O:39][CH3:38])=[C:41]([C:47]([F:50])([F:49])[F:48])[CH:42]=2)=[O:32])[CH:21]=[CH:20]3)[CH:11]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 682631,1'-CarbonyldiimidazoleHCID 6007055-Amino-2-methoxybenzotrifluorideHCID 593942601H-Indole, 5-[[6-[(phenylmethoxy)methyl]-4-pyrimidinyl]oxy]-

生成物 1

HCID 59394510HCID 59394510、化合物

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5-(6-(benzyloxymethyl)pyrimidin-4-yloxy)-1H-indole (0.8 g, 2.41 mmol) in 35 mL of DCE, CDI (1.17 g, 7.24 mmol) is added followed by TEA (1 mL, 7.24 mmol). Mixture is stirred at rt overnight and then 4-methoxy-3-(trifluoromethyl)aniline (1.38 g, 7.24 mmol) is added followed by stirring for 4 days. The reaction is diluted with DCM, washed with saturated aqueous NaHCO3 (×2), brine, and the organic layer is dried over Na2SO4. After concentration, the residue is purified by FCC (5-60% EtOAc/heptane) to give the title compound. MS (ESI) m/z 549.1 (M+1).

後処理

  1. stirringby stirring for 4 days
  2. washwashed with saturated aqueous NaHCO3 (×2), brine
  3. dry with materialthe organic layer is dried over Na2SO4
  4. concentrationAfter concentration
  5. customthe residue is purified by FCC (5-60% EtOAc/heptane)

出典と根拠

ORDレコード
ord-5f07ad80665e4cda83646908f72ce0a4
出典データセット
uspto-grants-2013_09
特許番号
US08541432B2

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