2,6-Lutidine → HCID 86652692、化合物

HRID 2095522

反応式

HRID 2095522 の反応式
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[C:5]([CH:7]=[CH:8][C:9]=1[C:10]([F:13])([F:12])[F:11])[NH2:6].Br[CH:17]([CH3:23])[C:18]([O:20][CH2:21][CH3:22])=[O:19].N1C(C)=CC=CC=1C>C(#N)C>[CH2:21]([O:20][C:18](=[O:19])[CH:17]([NH:6][C:5]1[CH:7]=[CH:8][C:9]([C:10]([F:11])([F:12])[F:13])=[C:3]([C:2]([F:14])([F:15])[F:1])[CH:4]=1)[CH3:23])[CH3:22]

参加物

5

反応物 3

HCID 79372,6-Lutidine3 回HCID 79040Ethyl 2-bromopropionate3 回HCID 15485793,4-Bis(trifluoromethyl)aniline

生成物 1

HCID 86652692HCID 86652692、化合物収率 49%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

In analogy to intermediate 40B, 3,4-bis(trifluoromethyl)aniline and ethyl 2-bromopropionate with 2,6-lutidine were heated for 20 h at 82° C., diluted with acetonitrile and treated with 1 equivalent of ethyl 2-bromopropionate and 2,6-lutidine and refluxed for 2 days, treated again with 1 equivalent of ethyl 2-bromopropionate and 2,6-lutidine and continued to reflux for 2 days. Workup and purification by flash silica gel column (n-heptane/ethyl acetate 9:1 to 2:1) yielded 49% of the titled compound as yellow oil. MS: 328.08 (M−H−).

後処理

  1. temperaturerefluxed for 2 days
  2. temperatureto reflux for 2 days
  3. customWorkup and purification by flash silica gel column (n-heptane/ethyl acetate 9:1 to 2:1)

出典と根拠

ORDレコード
ord-6f8ee845b05c404b896f0b54c7f716e9
出典データセット
uspto-grants-2013_05
特許番号
US08445674B2

関連ノート

読み込み中…