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

HRID 321990ノート

反応式

HRID 321990 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-7be63c5bd358412eadf060c3f72230a0
出典データセット
uspto-grants-2001_04
特許番号
US06211178B1

反応ノート

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