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Triethylamine → N-[4-[(5,6,7,8-Tetrahydro-4H-thieno[3,2-b]azepin-4-yl)carbonyl]phenyl]-3,4-dichlorobenzamide

HRID 1939211
ノート
印刷プレビュー

反応式

HRID 1939211 の反応式
[NH2:1][C:2]1[CH:19]=[CH:18][C:5]([C:6]([N:8]2[CH2:14][CH2:13][CH2:12][CH2:11][C:10]3[S:15][CH:16]=[CH:17][C:9]2=3)=[O:7])=[CH:4][CH:3]=1.C(N(CC)CC)C.[Cl:27][C:28]1[CH:29]=[C:30]([CH:34]=[CH:35][C:36]=1[Cl:37])[C:31](Cl)=[O:32]>ClCCl>[S:15]1[C:10]2[CH2:11][CH2:12][CH2:13][CH2:14][N:8]([C:6]([C:5]3[CH:4]=[CH:3][C:2]([NH:1][C:31](=[O:32])[C:30]4[CH:34]=[CH:35][C:36]([Cl:37])=[C:28]([Cl:27])[CH:29]=4)=[CH:19][CH:18]=3)=[O:7])[C:9]=2[CH:17]=[CH:16]1
参加物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 8471TriethylamineHCID 76403Benzoyl chloride, 3,4-dichloro-HCID 214671424-(4-Aminobenzoyl)-5,6,7,8-tetrahydro-4H-thieno[3,2-b]azepine

生成物 1

HCID 21467135N-[4-[(5,6,7,8-Tetrahydro-4H-thieno[3,2-b]azepin-4-yl)carbonyl]phenyl]-3,4-dichlorobenzamide収率 51.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 0.30 g of 4-(4-aminobenzoyl)-5,6,7,8-tetrahydro-4H-thieno[3,2-b]azepine and 0.208 ml of triethylamine in 10 ml of dichloromethane is added, under argon, 0.251 g of 3,4-dichlorobenzoyl chloride. The mixture is stirred overnight and concentrated to dryness under vacuum. The residue is dissolved in ethyl acetate and the solution washed with H2O, 2N citric acid, NaHCO3 solution, brine and dried (Na2SO4). The solvent is removed and the residual yellow solid crystallized from ethyl acetate-hexane to give 0.254 g of crystals, m.p. 154°-160° C.

後処理

  1. concentrationconcentrated to dryness under vacuum
  2. dissolutionThe residue is dissolved in ethyl acetate
  3. washthe solution washed with H2O, 2N citric acid, NaHCO3 solution, brine
  4. dry with materialdried (Na2SO4)
  5. customThe solvent is removed
  6. customthe residual yellow solid crystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-f73a0e34a412472680a1d600fa5249b0
出典データセット
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05696112

反応ノート

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