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2-(1-Imidazolyl)-2-(4-chloro-methyl-1,3-dithiolan-2-ylidene)acetonitrile → 2-(1-Imidazolyl)-2-(4-methylidene-1,3-dithiolan-2-ylidene)acetonitrile

HRID 980217
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인쇄 미리보기

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HRID 980217 반응식
[N:1]1([C:6](=[C:9]2[S:13][C:12]([CH3:15])(Cl)[CH2:11][S:10]2)[C:7]#[N:8])[CH:5]=[CH:4][N:3]=[CH:2]1>O1CCCC1>[N:1]1([C:6](=[C:9]2[S:13][C:12](=[CH2:15])[CH2:11][S:10]2)[C:7]#[N:8])[CH:5]=[CH:4][N:3]=[CH:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 867412112-(1-Imidazolyl)-2-(4-chloro-methyl-1,3-dithiolan-2-ylidene)acetonitrile

생성물 1

HCID 537472672-(1-Imidazolyl)-2-(4-methylidene-1,3-dithiolan-2-ylidene)acetonitrile수율 79.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In 10 ml of tetrahydrofuran were dissolved 0.52 g (0.002 mole) of the 2-(1-imidazolyl)-2-(4-chloro- methyl-1,3-dithiolan-2-ylidene)acetonitrile obtained in Example 2 and 0.31 g of 1,8-diazabicyclo-[5,4,0]-7-undecene, and the reaction was carried out with heating under reflux for 1 hour. After the reaction solution was allowed to cool, the deposited salt was separated by filtration and the filtrate was concentrated to obtain crude crystals, which were then recrystallized from ethyl acetate-n-hexane to obtain 0.35 g of the desired compound in the form of crystals: melting point 115.7° C., yield 79%.

후처리

  1. temperaturewith heating
  2. temperatureunder reflux for 1 hour
  3. temperatureto cool
  4. customthe deposited salt was separated by filtration
  5. concentrationthe filtrate was concentrated
  6. customto obtain crude crystals, which
  7. customwere then recrystallized from ethyl acetate-n-hexane

출처 및 근거

ORD 기록
ord-5b257539b3ba4f76b7284bd6668c913d
출처 데이터셋
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04636519

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