Dimethylformamide diethylacetal → 7-benzyl-octahydro-5H,9bH-2a,4a,7,9a-tetraazacycloocta[cd]pentalene

HRID 1735937

反応式

HRID 1735937 の反応式
[CH2:1]([N:8]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15][NH:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:20](OC(OCC)N(C)C)C>C1C=CC=CC=1>[CH2:1]([N:8]1[CH2:19][CH2:18][N:17]2[CH2:16][CH2:15][N:14]3[CH2:13][CH2:12][N:11]([CH:20]23)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 70913Dimethylformamide diethylacetalHCID 100840821-Benzyl-1,4,7,10-tetraazacyclododecane

生成物 1

HCID 109676597-benzyl-octahydro-5H,9bH-2a,4a,7,9a-tetraazacycloocta[cd]pentalene収率 96%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of 1-benzyl-1,4,7,10-tetraazacyclododecane (4 g; 0.015 mol ) and dimethylformamide diethylacetal (6.88 g; 0.0467 mol) in benzene (40 ml ) is heated at 80° C. and the azeotropic mixture ethanol-benzene is distilled away. When the conversion is ended, the solvent is evaporated under reduced pressure and the final product is obtained as a yellow oil (4.0 g). Yield 96%

後処理

  1. distillationthe azeotropic mixture ethanol-benzene is distilled away
  2. customthe solvent is evaporated under reduced pressure

出典と根拠

ORDレコード
ord-7d675e993b774ab085c1fd7e83b991ea
出典データセット
uspto-grants-1996_07
特許番号
US05539105

関連ノート

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