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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
ノート
印刷プレビュー

反応式

HRID 980217 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-5b257539b3ba4f76b7284bd6668c913d
出典データセット
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04636519

反応ノート

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