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

HRID 321990노트

반응식

HRID 321990 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene촉매HCID 6342Acetonitrile용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-7be63c5bd358412eadf060c3f72230a0
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211178B1

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