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Ammonia → HCID 178508663、化合物

HRID 1195418
ノート
印刷プレビュー

反応式

HRID 1195418 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([C:12]#[N:13])[C:6]([C:14]#[N:15])=[CH:5]2.C[O-].[Na+].[Na].[NH3:20]>CO>[Br:1][C:2]1[CH:11]=[CH:10][C:9]2=[CH:8][C:7]3[C:12](=[NH:13])[NH:15][C:14](=[NH:20])[C:6]=3[CH:5]=[C:4]2[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 222AmmoniaHCID 7847106-Bromo-2,3-dicyanonaphthaleneHCID 5360545SodiumHCID 10942334Sodium Methoxide

生成物 1

HCID 178508663HCID 178508663、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

Under nitrogen, 44.1 g (0.17 mol) of 6-bromo-2,3-dicyanonaphthalene was added to a solution of sodium methoxide in methanol prepared by adding 1.92 g (84 mmols) of metallic sodium in 5 times to 270 ml of absolute methanol, and anhydrous ammonia gas was slowly bubbled into the resulting mixture with sufficient mixing at room temperature for about 1 hour. The mixture was refluxed for about 3 hours, while bubbling therethrough anhydrous ammonia gas. After cooling, the yellow solid precipitated was collected by filtration, sufficiently washed with methanol and dried under reduced pressure to obtain 45 g of 6-bromo-1,3-diiminobenz[f]isoindoline as a yellow solid. IR spectrum of this 6-bromo-1,3-diiminobenz[f]isoindoline is shown in FIG. 4. The 6-bromo-1,3-diiminobenz[f]isoindoline was used in the subsequent reaction without further purification.

後処理

  1. customprepared
  2. customwas slowly bubbled into the resulting mixture
  3. additionwith sufficient mixing at room temperature for about 1 hour
  4. temperatureThe mixture was refluxed for about 3 hours
  5. customwhile bubbling
  6. temperatureAfter cooling
  7. customthe yellow solid precipitated
  8. filtrationwas collected by filtration
  9. washsufficiently washed with methanol
  10. customdried under reduced pressure

出典と根拠

ORDレコード
ord-fbbbcf9d192b4383aa81762b2f285be0
出典データセット
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05110968

反応ノート

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