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(Methylthio)acetic acid → N-[2-chloro-4-[5-(3,4,5-trichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]phenyl]methyl-2-(methylthio) acetamide

HRID 1880237
ノート
印刷プレビュー

反応式

HRID 1880237 の反応式
[NH2:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:13][C:12]([C:18]3[CH:23]=[C:22]([Cl:24])[C:21]([Cl:25])=[C:20]([Cl:26])[CH:19]=3)([C:14]([F:17])([F:16])[F:15])[O:11][N:10]=2)=[CH:5][C:4]=1[Cl:27].[CH3:28][S:29][CH2:30][C:31](O)=[O:32].Cl.CN(C)CCCN=C=NCC.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl.C(N(CC)CC)C>[Cl:27][C:4]1[CH:5]=[C:6]([C:9]2[CH2:13][C:12]([C:18]3[CH:23]=[C:22]([Cl:24])[C:21]([Cl:25])=[C:20]([Cl:26])[CH:19]=3)([C:14]([F:17])([F:16])[F:15])[O:11][N:10]=2)[CH:7]=[CH:8][C:3]=1[CH2:2][NH:1][C:31](=[O:32])[CH2:30][S:29][CH3:28]
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 75551(Methylthio)acetic acidHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 446282993-(4-Aminomethyl-3-chlorophenyl)-5-(3,4,5-trichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole

生成物 1

HCID 49763421N-[2-chloro-4-[5-(3,4,5-trichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]phenyl]methyl-2-(methylthio) acetamide

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 8471Triethylamine溶媒

実験手順

To a solution of 0.11 g of 3-(4-aminomethyl-3-chlorophenyl)-5-(3,4,5-trichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole, 0.051 g of (methylthio) acetic acid and 0.048 g of triethylamine in 2 mL of chloroform, 0.092 g of 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride was added and the resultant mixture was stirred at room temperature for 15 hours. After the completion of the reaction, 2 mL of a saturated sodium hydrogen carbonate aqueous solution was added to the reaction mixture and the organic phase was separated off, followed by purifying the organic phase as it was by preparative medium pressure liquid chromatography eluting with ethyl acetate-hexane (a gradient from 1:4 to 1:1) using a medium pressure preparative apparatus (trade name: YFLC-Wprep; manufactured by Yamazen Corporation) to obtain 0.12 g of the objective substance as a colorless resinoid.

後処理

  1. additionwas added to the reaction mixture
  2. customthe organic phase was separated off
  3. customby purifying the organic phase as it
  4. washeluting with ethyl acetate-hexane (a gradient from 1:4 to 1:1)
  5. customto obtain 0.12 g of the objective substance as a colorless resinoid

出典と根拠

ORDレコード
ord-94d6b82d4c6747d9aab98e30b239e20e
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08318757B2

反応ノート

読み込み中…

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