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Potassium Iodide → 2',5-dichloro-2-(3-carbobenzoxyaminomethyl-5-diethylaminomethyl-4H-1,2,4-triazol-4-yl)-benzophenone

HRID 614057
ノート
印刷プレビュー

反応式

HRID 614057 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[O:35])[C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[N:16]1[C:20]([CH2:21]Cl)=[N:19][N:18]=[C:17]1[CH2:23][NH:24][C:25]([O:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)=[O:26].[I-].[K+].[CH2:38]([NH:40][CH2:41][CH3:42])[CH3:39]>CO.C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[O:35])[C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[N:16]1[C:20]([CH2:21][N:40]([CH2:41][CH3:42])[CH2:38][CH3:39])=[N:19][N:18]=[C:17]1[CH2:23][NH:24][C:25]([O:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)=[O:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 4875Potassium IodideHCID 8021DiethylamineHCID 15573091HCID 15573091、化合物

生成物 1

HCID 213256792',5-dichloro-2-(3-carbobenzoxyaminomethyl-5-diethylaminomethyl-4H-1,2,4-triazol-4-yl)-benzophenone

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6212Chloroform
溶媒

実験手順

To a solution of 2',5-dichloro-2-(3-carbobenzoxyaminomethyl-5-chloromethyl-4H-1,2,4-triazol-4-yl)-benzophenone (1.32 g) in methanol (20 ml) and chloroform (20 ml), potassium iodide (0.4 g) and diethylamine (3 ml) are added, and the resultant mixture is refluxed for 5 hours. The reaction mixture is evaporated under reduced pressure to remove the solvent, and the residue is extracted with ethyl acetate. The ethyl acetate layer is washed with water, dried, and evaporated under reduced pressure to remove the ethyl acetate. The residue is treated with ether to give 2',5-dichloro-2-(3-carbobenzoxyaminomethyl-5-diethylaminomethyl-4H-1,2,4-triazol-4-yl)-benzophenone (1.1 g). The product is recrystallized from ether-ethyl acetate to give crystals melting at 89° to 94° C.

後処理

  1. customThe reaction mixture is evaporated under reduced pressure
  2. customto remove the solvent
  3. extractionthe residue is extracted with ethyl acetate
  4. washThe ethyl acetate layer is washed with water
  5. customdried
  6. customevaporated under reduced pressure
  7. customto remove the ethyl acetate
  8. additionThe residue is treated with ether

出典と根拠

ORDレコード
ord-7be09fac36704b04b599a9b75b2994db
出典データセット
uspto-grants-1979_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04143048

反応ノート

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