2-Isocyanato-1,1-dimethoxyethane → 1-Benzylidene-2-[4-(4-chloro-alpha-cyanobenzyl)-3,5-dichlorophenyl]-4-(2,2-dimethoxyethyl)semicarbazide

HRID 1604315ノート

反応式

HRID 1604315 の反応式
[Cl:1][C:2]1[CH:27]=[CH:26][C:5]([CH:6]([C:9]2[C:14]([Cl:15])=[CH:13][C:12]([NH:16][N:17]=[CH:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[CH:11][C:10]=2[Cl:25])[C:7]#[N:8])=[CH:4][CH:3]=1.[CH3:28][O:29][CH:30]([O:35][CH3:36])[CH2:31][N:32]=[C:33]=[O:34]>C(#N)C.C1CCN2C(=NCCC2)CC1>[CH:18](=[N:17][N:16]([C:12]1[CH:11]=[C:10]([Cl:25])[C:9]([CH:6]([C:7]#[N:8])[C:5]2[CH:26]=[CH:27][C:2]([Cl:1])=[CH:3][CH:4]=2)=[C:14]([Cl:15])[CH:13]=1)[C:33]([NH:32][CH2:31][CH:30]([O:35][CH3:36])[O:29][CH3:28])=[O:34])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

参加物

5

反応物 2

HCID 154556412-Isocyanato-1,1-dimethoxyethaneHCID 86754869Benzaldehyde 4-(4-chloro-alpha-cyanobenzyl)-3,5-dichlorophenyl hydrazone

生成物 1

HCID 543848701-Benzylidene-2-[4-(4-chloro-alpha-cyanobenzyl)-3,5-dichlorophenyl]-4-(2,2-dimethoxyethyl)semicarbazide収率 87.8%

試薬・触媒・溶媒 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene触媒HCID 6342Acetonitrile溶媒

実験手順

In 20 ml of acetonitrile was suspended 3.2 g of benzaldehyde 4-(4-chloro-α-cyanobenzyl)-3,5-dichlorophenyl hydrazone. To the suspension were added 1.5 g of 2,2-dimethoxyethyl isocyanate and 20 mg of DBU. The reaction was allowed to proceed for one hour at room temperature, then the resulting crystalline precipitate was collected by filtration, which was washed with hexane, followed by drying to afford 3.7 g of the titled compound as colorless crystals, m.p. 190-191° C.

後処理

  1. filtrationthe resulting crystalline precipitate was collected by filtration, which
  2. washwas washed with hexane
  3. customby drying

出典と根拠

ORDレコード
ord-a16d40e651f7413188d77af635a281ab
出典データセット
uspto-grants-1999_11
特許番号
US05994355

反応ノート

読み込み中…