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Ammonia → HCID 178508663、化合物

HRID 1755702
ノート
印刷プレビュー

反応式

HRID 1755702 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 to 270 ml of absolute methanol in 5 times, and anhydrous ammonia gas was slowly bubbled into the resulting mixture with sufficient stirring 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 filtered and the residue was 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. temperatureThe mixture was refluxed for about 3 hours
  4. customwhile bubbling
  5. temperatureAfter cooling
  6. customthe yellow solid precipitated
  7. filtrationwas filtered
  8. washthe residue was sufficiently washed with methanol
  9. customdried under reduced pressure

出典と根拠

ORDレコード
ord-7546540cbf5e4b7793864c8c20e27222
出典データセット
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05438135

反応ノート

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