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Bis(2,2,2-trichloroethyl) hydrazine-1,2-dicarboxylate → Bis(2,2,2-trichloroethyl) 1-(2,3-dihydrobenzofuran-5-yl)hydrazine-1,2-dicarboxylate

HRID 384308
ノート
印刷プレビュー

反応式

HRID 384308 の反応式
O1C2C=CC=CC=2CC1.[O:10]1[C:14]2[CH:15]=[CH:16][C:17]([N:19]([C:29]([O:31][CH2:32][C:33]([Cl:36])([Cl:35])[Cl:34])=[O:30])[NH:20][C:21]([O:23][CH2:24][C:25]([Cl:28])([Cl:27])[Cl:26])=[O:22])=[CH:18][C:13]=2[CH2:12][CH2:11]1.N(C(OCC(Cl)(Cl)Cl)=O)NC(OCC(Cl)(Cl)Cl)=O>ClCCl.[Cl-].[Zn+2].[Cl-]>[O:10]1[C:14]2[CH:15]=[CH:16][C:17]([N:19]([C:29]([O:31][CH2:32][C:33]([Cl:34])([Cl:35])[Cl:36])=[O:30])[NH:20][C:21]([O:23][CH2:24][C:25]([Cl:27])([Cl:28])[Cl:26])=[O:22])=[CH:18][C:13]=2[CH2:12][CH2:11]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 2

HCID 350435Bis(2,2,2-trichloroethyl) hydrazine-1,2-dicarboxylateHCID 86648897Bis(2,2,2-trichloroethyl) 1-(2,3-dihydrobenzofuran-5-yl)hydrazine-1,2-dicarboxylate 2,3-Dihydro-benzofuran

生成物 1

HCID 10505571Bis(2,2,2-trichloroethyl) 1-(2,3-dihydrobenzofuran-5-yl)hydrazine-1,2-dicarboxylate収率 96.6%

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒
HCID 6344
Dichloromethane
溶媒

実験手順

Bis(2,2,2-trichloroethyl) 1-(2,3-dihydrobenzofuran-5-yl)hydrazine-1,2-dicarboxylate 2,3-Dihydro-benzofuran 7a (0.6 mL, 5.32 mmol), bis(2,2,2-trichloroethyl) hydrazine-1,2-dicarboxylate (1.96 g, 5.15 mmol) and zinc chloride (920 mg, 6.76 mmol) were dissolved in 40 mL of dichloromethane. The reaction was reacted overnight at room temperature and monitored by TLC until the disappearance of the starting materials. Then the mixture was purified by silica gel column chromatography to obtain the title compound bis(2,2,2-trichloroethyl) 1-(2,3-dihydrobenzofuran-5-yl)hydrazine-1,2-dicarboxylate 7b (2.5 g, yield 96.6%) as a white solid.

後処理

  1. customThe reaction was reacted overnight at room temperature
  2. customThen the mixture was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-3a13d733d8684b419f183f2627834bef
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367710B2

反応ノート

読み込み中…

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