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Diisopropyl Ether → HCID 22492912、化合物

HRID 1816352
ノート
印刷プレビュー

反応式

HRID 1816352 の反応式
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[CH:8]1([N:14]2[CH2:19][CH2:18][CH:17]([C:20]3[CH:25]=[CH:24][C:23]([C:26]4[S:30][C:29]([NH2:31])=[N:28][N:27]=4)=[CH:22][CH:21]=3)[CH2:16][CH2:15]2)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.Br[CH2:33][C:34]([C:36]1[CH:46]=[CH:45][C:39]([C:40]([O:42][CH2:43][CH3:44])=[O:41])=[CH:38][CH:37]=1)=O.C(OC(C)C)(C)C>C(O)C>[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[CH:8]1([N:14]2[CH2:15][CH2:16][CH:17]([C:20]3[CH:25]=[CH:24][C:23]([C:26]4[S:30][C:29]5=[N:31][C:34]([C:36]6[CH:46]=[CH:45][C:39]([C:40]([O:42][CH2:43][CH3:44])=[O:41])=[CH:38][CH:37]=6)=[CH:33][N:28]5[N:27]=4)=[CH:22][CH:21]=3)[CH2:18][CH2:19]2)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7914Diisopropyl EtherHCID 11966043Ethyl 4-(2-bromoacetyl)benzoateHCID 22492898HCID 22492898、化合物

生成物 1

HCID 22492912HCID 22492912、化合物収率 41.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

A mixture of 5-[4-(1-cyclohexyl-4-piperidyl)phenyl]-1,3,4-thiadiazol-2-amine trifluoroacetate (0.78 g) and ethyl 4-(bromoacetyl)benzoate (0.6 g) in ethanol (15 ml) was stirred for 5 hours at 80° C. After being cooled to room temperature, the reaction mixture was poured into isopropyl ether. The resulting precipitate was collected by filtration, washed with isopropyl ether and added to a solution of trifluoroacetic acid (1.5 ml) in xylene (15 ml). Then a mixture was stirred for 3 hours at 130° C. After being cooled to room temperature, the reaction mixture was poured into isopropyl ether. The resulting precipitate was collected by filtration and washed with isopropyl ether to give ethyl 4-[2-[4-(1-cyclohexyl-4-piperidyl)phenyl]imidazo[2,1-b][1,3,4]thiadiazol-6-yl]benzoate trifluroacetate (0.45 g).

後処理

  1. temperatureAfter being cooled to room temperature
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with isopropyl ether
  4. additionadded to a solution of trifluoroacetic acid (1.5 ml) in xylene (15 ml)
  5. stirringThen a mixture was stirred for 3 hours at 130° C
  6. temperatureAfter being cooled to room temperature
  7. additionthe reaction mixture was poured into isopropyl ether
  8. filtrationThe resulting precipitate was collected by filtration
  9. washwashed with isopropyl ether

出典と根拠

ORDレコード
ord-95ce74ad59c943d3aa0c6eb056a6af4e
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06884774B2

反応ノート

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