Triethylamine → 4-[2,5-Dioxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4,5,6,7,8-octahydro-quinazolin-4-yl]-3-methylsulfanyl-benzonitrile

HRID 59645ノート

反応式

HRID 59645 の反応式
C(N(CC)CC)C.Cl.[NH2:9][CH:10]([C:21]1[C:26](=[O:27])[CH2:25][CH2:24][CH2:23][C:22]=1[NH:28][C:29]1[CH:34]=[CH:33][CH:32]=[C:31]([C:35]([F:38])([F:37])[F:36])[CH:30]=1)[C:11]1[CH:18]=[CH:17][C:14]([C:15]#[N:16])=[CH:13][C:12]=1[S:19][CH3:20].[C:39](N1C=CN=C1)(N1C=CN=C1)=[O:40]>C(#N)C>[O:40]=[C:39]1[NH:9][CH:10]([C:11]2[CH:18]=[CH:17][C:14]([C:15]#[N:16])=[CH:13][C:12]=2[S:19][CH3:20])[C:21]2[C:26](=[O:27])[CH2:25][CH2:24][CH2:23][C:22]=2[N:28]1[C:29]1[CH:34]=[CH:33][CH:32]=[C:31]([C:35]([F:38])([F:36])[F:37])[CH:30]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 1186928904-{Amino-[6-oxo-2-(3-trifluoromethyl-phenylamino)-cyclohex-1-enyl]-methyl}-3-methylsulfanyl-benzonitrile hydrochloride2 回

生成物 1

HCID 1186929024-[2,5-Dioxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4,5,6,7,8-octahydro-quinazolin-4-yl]-3-methylsulfanyl-benzonitrile

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Triethylamine (89 μL, 0.634 mmol) is added to a mixture of 4-{amino-[6-oxo-2-(3-trifluoromethyl-phenylamino)-cyclohex-1-enyl]-methyl}-3-methylsulfanyl-benzonitrile hydrochloride (INTERMEDIATE 5, 1.19 g, 2.54 mmol) and 1,1′-carbonyldiimidazole (480 mg, 2.96 mmol) in acetonitrile (4 mL) and the mixture is stirred at room temperature for 15 min. The reaction mixture is evaporated. Water is added, the precipitate is filtered and washed with water. The residue is dissolved in dichloromethane and evaporated. Yield: 1.02 g. ESI mass spectrum: [M+H]+=458; Retention time HPLC: 1.05 min (Z018_S04).

後処理

  1. customThe reaction mixture is evaporated
  2. additionWater is added
  3. filtrationthe precipitate is filtered
  4. washwashed with water
  5. dissolutionThe residue is dissolved in dichloromethane
  6. customevaporated
  7. custom1.05 min (Z018_S04)

出典と根拠

ORDレコード
ord-b63f83b7084342aab5e71bb433695c13
出典データセット
uspto-grants-2016_09
特許番号
US09440930B2

反応ノート

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