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Hydrochloric Acid → HCID 15434939, 화합물

HRID 1604319
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HRID 1604319 반응식
[CH:1](=[N:8][N:9]([C:19]1[CH:24]=[C:23]([Cl:25])[C:22]([CH:26]([C:34]#[N:35])[C:27]2[CH:32]=[CH:31][C:30]([Cl:33])=[CH:29][CH:28]=2)=[C:21]([Cl:36])[CH:20]=1)[C:10]([NH:12]CC(OC)OC)=[O:11])[C:2]1C=CC=CC=1.Cl>C(#N)C>[Cl:33][C:30]1[CH:29]=[CH:28][C:27]([CH:26]([C:22]2[C:23]([Cl:25])=[CH:24][C:19]([N:9]3[C:10](=[O:11])[NH:12][CH2:2][CH:1]=[N:8]3)=[CH:20][C:21]=2[Cl:36])[C:34]#[N:35])=[CH:32][CH:31]=1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 543848701-Benzylidene-2-[4-(4-chloro-alpha-cyanobenzyl)-3,5-dichlorophenyl]-4-(2,2-dimethoxyethyl)semicarbazide

생성물 1

HCID 15434939HCID 15434939, 화합물수율 91.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

In 30 ml of acetonitrile was suspended 3.5 g of 1-benzylidene-2-[4-(4-chloro-α-cyanobenzyl)-3,5-dichlorophenyl]-4-(2,2-dimethoxyethyl)semicarbazide produced in Working Example 2. To the suspension was added 0.7 g of 35% hydrochloric acid, and the reaction was allowed to proceed for one hour at room temperature. After completion of the reaction, the reaction mixture was cooled for 30 minutes at temperatures ranging from 0 to 10° C., then resulting crystalline precipitate was collected by filtration to afford 2.3 g of the titled compound as colorless crystals, m.p. 166-167° C.

후처리

  1. customproduced in Working Example 2
  2. customAfter completion of the reaction
  3. temperaturethe reaction mixture was cooled for 30 minutes at temperatures
  4. customranging from 0 to 10° C.
  5. filtrationresulting crystalline precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-773eace241964894b0a17edec7eb2083
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05994355

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