Water → 1-((4-Cyano-2-fluorophenyl)(2-ethoxy-6-oxocyclohex-1-enyl)methyl)-3-(3-(trifluoromethyl)phenyl)urea

HRID 517209ノート

反応式

HRID 517209 の反応式
F[B-](F)(F)F.C([O+:8]([CH2:11][CH3:12])[CH2:9][CH3:10])C.[C:13]([C:15]1[CH:20]=[CH:19][C:18]([CH:21]([C:36]2C(=O)C[CH2:39][CH2:38][C:37]=2[OH:43])[NH:22][C:23]([NH:25][C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([C:32]([F:35])([F:34])[F:33])[CH:27]=2)=[O:24])=[C:17]([F:44])[CH:16]=1)#[N:14].C(N(CC)C(C)C)(C)C.O>ClCCl>[C:13]([C:15]1[CH:20]=[CH:19][C:18]([CH:21]([C:36]2[C:37](=[O:43])[CH2:38][CH2:39][CH2:12][C:11]=2[O:8][CH2:9][CH3:10])[NH:22][C:23]([NH:25][C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([C:32]([F:33])([F:34])[F:35])[CH:27]=2)=[O:24])=[C:17]([F:44])[CH:16]=1)#[N:14]

参加物

6

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 2723982Triethyloxonium tetrafluoroborateHCID 867323291-((4-Cyano-2-fluorophenyl)(2-hydroxy-6-oxocyclohex-1-enyl)methyl)-3-(3-(trifluoromethyl)phenyl)urea2 回

生成物 1

HCID 867323301-((4-Cyano-2-fluorophenyl)(2-ethoxy-6-oxocyclohex-1-enyl)methyl)-3-(3-(trifluoromethyl)phenyl)urea

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Triethyloxonium tetrafluoroborate (1.60 g, 8.42 mmol) is added to a solution of 1-((4-cyano-2-fluorophenyl)(2-hydroxy-6-oxocyclohex-1-enyl)methyl)-3-(3-(trifluoromethyl)phenyl)urea (intermediate 40 1.80 g, 4.02 mmol) and N,N-diisopropylethylamine (1.60 mL, 9.2 mmol) in dichloromethane (15 mL), and the mixture is stirred at room temperature for 20 min Water is added, and the phases are separated. The organic layer is dried over Na2SO4 and concentrated under reduced pressure. Yield: 1.82 g; ESI mass spectrum [M+H]+=476, Retention time HPLC: 1.11 min (Z018_S04).

後処理

  1. additionis added
  2. customthe phases are separated
  3. dry with materialThe organic layer is dried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. custom1.11 min (Z018_S04)

出典と根拠

ORDレコード
ord-aefe943f0c6f43ca8b1189f41dff24a5
出典データセット
uspto-grants-2015_08
特許番号
US09115093B2

反応ノート

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