Sodium Azide → 6-(Azidomethyl)phenanthridine

HRID 718739ノート

反応式

HRID 718739 の反応式
[N-:1]=[N+:2]=[N-:3].[Na+].Br[CH2:6][C:7]1[N:8]=[C:9]2[C:14](=[C:15]3[C:20]=1[CH:19]=[CH:18][CH:17]=[CH:16]3)[CH:13]=[CH:12][CH:11]=[CH:10]2>CC(C)=O>[N:1]([CH2:6][C:7]1[N:8]=[C:9]2[C:14](=[C:15]3[C:20]=1[CH:19]=[CH:18][CH:17]=[CH:16]3)[CH:13]=[CH:12][CH:11]=[CH:10]2)=[N+:2]=[N-:3]

参加物

4

反応物 2

HCID 33557Sodium AzideHCID 856742386-(Bromomethyl)phenanthridine

生成物 1

HCID 867124836-(Azidomethyl)phenanthridine

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Sodium azide (715 mg, 11.0 mmol) was added to a solution of the bromide 6 (301 mg, 1.10 mmol) in dry acetone (30 mL). The reaction mixture was stirred at ambient temperature for 1 hour, then heated to reflux for 2 hours. The reaction mixture was then allowed to cool to room temperature, the excess sodium azide was filtered off, and the solvent was removed under reduced pressure to yield the crude azide 7 as a light yellow crystalline solid, which was used immediately in the next step without further purification.

後処理

  1. temperatureheated
  2. temperatureto reflux for 2 hours
  3. temperatureto cool to room temperature
  4. filtrationthe excess sodium azide was filtered off
  5. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-db77acfd88524a279d5592adb1161c74
出典データセット
uspto-grants-2015_11
特許番号
US09194802B2

反応ノート

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