2-Butanamine, 2-methyl- → 3-Cyclohexyl-5-ethoxy-1,3-dihydro-1-[2-methoxy-4-[N-(1,1-dimethylpropyl)carbamoyl]benzyl]-2H-benzimidazol-2-one

HRID 2258545ノート

反応式

HRID 2258545 の反応式
[C:1]([NH:5][C:6]([C:8]1[CH:33]=[CH:32][C:11]([CH2:12][N:13]2[C:17]3[CH:18]=[CH:19][C:20]([O:22][CH2:23][CH3:24])=[CH:21][C:16]=3[N:15]([CH:25]3[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]3)[C:14]2=[O:31])=[C:10]([O:34][CH3:35])[CH:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=C[C:46]=2N=N1.CCN(C(C)C)C(C)C.C(N)(CC)(C)C>C(Cl)Cl>[CH:25]1([N:15]2[C:16]3[CH:21]=[C:20]([O:22][CH2:23][CH3:24])[CH:19]=[CH:18][C:17]=3[N:13]([CH2:12][C:11]3[CH:32]=[CH:33][C:8]([C:6](=[O:7])[NH:5][C:1]([CH3:4])([CH3:2])[CH2:3][CH3:46])=[CH:9][C:10]=3[O:34][CH3:35])[C:14]2=[O:31])[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1

参加物

6

反応物 4

HCID 689862-Butanamine, 2-methyl-HCID 81531DiisopropylethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 229224911-[4-(N-tert-Butylcarbamoyl)-2-methoxybenzyl]-3-cyclohexyl-5-ethoxy-1,3-dihydro-2H-benzimidazol-2-one

生成物 1

HCID 229225423-Cyclohexyl-5-ethoxy-1,3-dihydro-1-[2-methoxy-4-[N-(1,1-dimethylpropyl)carbamoyl]benzyl]-2H-benzimidazol-2-one収率 36.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 0.9 g of the compound obtained in Example 15 Step B, 0.9 g of BOP and 1 ml of DIPEA in 20 ml of DCM is added 1 g of tert-amylamine, and the mixture is left stirring for 3 hours at RT. The reaction mixture is washed with 1N HCl solution, with 1N NaOH solution and dried over Na2SO4, and the solvent is evaporated off under vacuum. The residue is chromatographed on silica, eluting with DCM. 0.34 g of the expected product is obtained, mp=164° C.

後処理

  1. waitthe mixture is left
  2. washThe reaction mixture is washed with 1N HCl solution, with 1N NaOH solution
  3. dry with materialdried over Na2SO4
  4. customthe solvent is evaporated off under vacuum
  5. customThe residue is chromatographed on silica
  6. washeluting with DCM

出典と根拠

ORDレコード
ord-f55ae4b4c20a4304814809370b70318a
出典データセット
uspto-grants-1997_08
特許番号
US05661169

反応ノート

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