Methyl (2E)-3-{3-fluoro-2-[(triphenylphosphoranylidene)amino]phenyl}propenoate → Methyl (2E)-3-{3-fluoro-2-[({[2-methoxy-5-(trifluoromethyl)phenyl]imino}methylene)amino]-phenyl}-2-propenoate

HRID 1893739

反応式

HRID 1893739 の反応式
[F:1][C:2]1[C:3]([N:14]=P(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=[C:4](/[CH:8]=[CH:9]/[C:10]([O:12][CH3:13])=[O:11])[CH:5]=[CH:6][CH:7]=1.[N:34]([C:37]1[CH:42]=[C:41]([C:43]([F:46])([F:45])[F:44])[CH:40]=[CH:39][C:38]=1[O:47][CH3:48])=[C:35]=O>ClCCl>[F:1][C:2]1[C:3]([N:14]=[C:35]=[N:34][C:37]2[CH:42]=[C:41]([C:43]([F:44])([F:46])[F:45])[CH:40]=[CH:39][C:38]=2[O:47][CH3:48])=[C:4](/[CH:8]=[CH:9]/[C:10]([O:12][CH3:13])=[O:11])[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 11983908Methyl (2E)-3-{3-fluoro-2-[(triphenylphosphoranylidene)amino]phenyl}propenoateHCID 11983909Benzene, 2-isocyanato-1-methoxy-4-(trifluoromethyl)-

生成物 1

HCID 86597232Methyl (2E)-3-{3-fluoro-2-[({[2-methoxy-5-(trifluoromethyl)phenyl]imino}methylene)amino]-phenyl}-2-propenoate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

5.0 g (10.98 mmol) of methyl (2E)-3-{3-fluoro-2-[(triphenylphosphoranylidene)amino]phenyl}-2-propenoate (Example 10A) are initially charged in 50 ml of dichloromethane, and the mixture is stirred with 2.5 g (11.53 mmol) of 2-isocyanato-1-methoxy-4-(trifluoromethyl)benzene (Example 17A) at room temperature overnight. The solvent is removed by distillation and the product is then purified by chromatography on silica gel (isohexane/dichloromethane 2:1; 1:1) and recrystallized from isohexane.

後処理

  1. customThe solvent is removed by distillation
  2. customthe product is then purified by chromatography on silica gel (isohexane/dichloromethane 2:1; 1:1)
  3. customrecrystallized from isohexane

出典と根拠

ORDレコード
ord-be11903d82474288b5bbb11a44c86ca9
出典データセット
uspto-grants-2013_08
特許番号
US08513255B2

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