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Diisopropyl Ether → HCID 22492950、化合物

HRID 1816327
ノート
印刷プレビュー

反応式

HRID 1816327 の反応式
I[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:12][C:11]([C:13]3[CH:18]=[CH:17][C:16]([N:19]4[CH2:24][CH2:23][N:22]([CH:25]5[CH2:30][CH2:29][CH:28]([CH3:31])[CH2:27][CH2:26]5)[CH2:21][CH2:20]4)=[CH:15][CH:14]=3)=[N:10][N:9]=2)=[CH:4][CH:3]=1.[CH:32]([O:34][CH2:35][CH3:36])=[O:33].C(O)C.[O-]CC.[Na+].C(OC(C)C)(C)C>CN(C=O)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:31][CH:28]1[CH2:29][CH2:30][CH:25]([N:22]2[CH2:23][CH2:24][N:19]([C:16]3[CH:17]=[CH:18][C:13]([C:11]4[S:12][C:8]([C:5]5[CH:6]=[CH:7][C:2]([C:32]([O:34][CH2:35][CH3:36])=[O:33])=[CH:3][CH:4]=5)=[N:9][N:10]=4)=[CH:14][CH:15]=3)[CH2:20][CH2:21]2)[CH2:26][CH2:27]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7914Diisopropyl EtherHCID 8025Ethyl formateHCID 22492909HCID 22492909、化合物HCID 23706232Ethanol sodium ethoxide

生成物 1

HCID 22492950HCID 22492950、化合物

試薬・触媒・溶媒 2

HCID 178418476HCID 178418476、化合物触媒
HCID 6228
Dimethylformamide
溶媒

実験手順

To a suspension of 1-[4-[5-(4-iodophenyl)-1,3,4-thiadiazol-2-yl]phenyl]-4-(4-methylcyclohexyl)piperazine (2 g) in DMF (40 ml) was successively added ethyl formate (0.56 ml), dichlorobis(triphenylphosphine)palladium(II) (0.52 g) and 20% sodium ethoxide ethanol solution (4.43 ml) with stirring and the mixture was stirred at 40° C. for 2 hours. The reaction mixture was added diisopropyl ether (600 ml). The resulting precipitate was collected by filtration. The precipitate was dissolved THF (200 ml), insoluble materials were filtered off and solution was concentrated in vacuo. The resulting residue was washed with acetonitrile, and dried to give ethyl 4-[5-[4-[4-(4-methylcyclohexyl)-1-piperazinyl]phenyl]-1,3,4-thiadiazol-2-yl]benzoate (1.07 g).

後処理

  1. stirringthe mixture was stirred at 40° C. for 2 hours
  2. filtrationThe resulting precipitate was collected by filtration
  3. dissolutionThe precipitate was dissolved THF (200 ml), insoluble materials
  4. filtrationwere filtered off
  5. concentrationsolution was concentrated in vacuo
  6. washThe resulting residue was washed with acetonitrile
  7. customdried

出典と根拠

ORDレコード
ord-ab64febad9a54cee84fea87e5c031566
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

読み込み中…

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