(e)-n-[4-(3-Bromo-propyl)-3-chloro-phenyl]-3-(2-chloro-4-trifluoromethyl-phenyl)-acrylamide → (e)-n-[3-Chloro-4-(3-diethylamino-propyl)-phenyl]-3-(2-chloro-4-trifluoromethyl-phenyl)-acrylamide

HRID 898631ノート

反応式

HRID 898631 の反応式
Br[CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:26])/[CH:13]=[CH:14]/[C:15]2[CH:20]=[CH:19][C:18]([C:21]([F:24])([F:23])[F:22])=[CH:17][C:16]=2[Cl:25])=[CH:7][C:6]=1[Cl:27]>C(NCC)C.CCOC(C)=O>[Cl:27][C:6]1[CH:7]=[C:8]([NH:11][C:12](=[O:26])/[CH:13]=[CH:14]/[C:15]2[CH:20]=[CH:19][C:18]([C:21]([F:24])([F:23])[F:22])=[CH:17][C:16]=2[Cl:25])[CH:9]=[CH:10][C:5]=1[CH2:4][CH2:3][CH2:2][N:11]([CH2:12][CH3:13])[CH2:8][CH3:7]

参加物

4

反応物 1

HCID 87610233(e)-n-[4-(3-Bromo-propyl)-3-chloro-phenyl]-3-(2-chloro-4-trifluoromethyl-phenyl)-acrylamide

生成物 1

HCID 59691692(e)-n-[3-Chloro-4-(3-diethylamino-propyl)-phenyl]-3-(2-chloro-4-trifluoromethyl-phenyl)-acrylamide

試薬・触媒・溶媒 2

HCID 8021Diethylamine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 0.290 g (0.603 mmol) (E)-N-[4-(3-bromo-propyl)-3-chloro-phenyl]-3-(2-chloro-4-trifluoromethyl-phenyl)-acrylamide (Z45d) in 2 mL diethylamine was heated to 100° C. in a sealed reaction vessel in the microwave for 5 min. The reaction mixture was diluted with EtOAc, the org. phase was washed with water, dried over sodium sulphate and evaporated down i. vac. The residue was triturated with ether, the precipitate was filtered off, washed with ether and dried in a HV.

後処理

  1. washphase was washed with water
  2. dry with materialdried over sodium sulphate
  3. customevaporated down i
  4. customThe residue was triturated with ether
  5. filtrationthe precipitate was filtered off
  6. washwashed with ether
  7. customdried in a HV

出典と根拠

ORDレコード
ord-a804382e0dbb42df9fcaf6cef49aebde
出典データセット
uspto-grants-2008_04
特許番号
US07351719B2

反応ノート

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