Sodium Nitrite → HCID 136331513、化合物

HRID 1097224ノート

反応式

HRID 1097224 の反応式
[NH2:1][C:2]1[CH:6]=[C:5]([C:7]([CH3:10])([CH3:9])[CH3:8])[Se:4][C:3]=1[C:11]([NH2:13])=[O:12].[N:14]([O-])=O.[Na+]>S(=O)(=O)(O)O>[C:7]([C:5]1[Se:4][C:3]2[C:11](=[O:12])[NH:13][N:14]=[N:1][C:2]=2[CH:6]=1)([CH3:10])([CH3:8])[CH3:9]

参加物

4

反応物 2

HCID 23668193Sodium NitriteHCID 866468893-Amino-5-tert-butylselenophene-2-carboxamide

生成物 1

HCID 136331513HCID 136331513、化合物収率 77%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

反応条件

温度
0 °C

実験手順

To an ice cold solution (0° C.) of 3-amino-5-(tert-butyl)selenophene-2-carboxamide (3.0 g, 12.2 mmol) in concentrated sulfuric acid (50 mL) was added a cold (0° C.) solution of sodium nitrite (0.92 g, 13.4 mmol) in concentrated sulfuric acid (10 mL) for 10 min (while adding, the temperature should keep between −5-0° C.). After addition, the mixture was stirred at 0° C. for 1 h and at rt for 1 h. The reaction mixture was cooled and poured into crushed ice slowly with stirring for 15 min and stirred at the same temperature for 15 min. The solid was filtered, washed with ice cold water and dried to give the product as a off-white color solid (2.4 g, 77%), mp 158-160° C. 1H NMR (400 MHz, CDCl3): δ 7.67 (1H, s, H-7), 1.50 (9H, s, tert-butyl); LC-MS (negative ion mode): m/z 254, 256 (M−H)—.

後処理

  1. additionwhile adding
  2. customshould keep between −5-0° C.
  3. additionAfter addition
  4. temperatureThe reaction mixture was cooled
  5. additionpoured
  6. custominto crushed ice slowly
  7. stirringwith stirring for 15 min
  8. stirringstirred at the same temperature for 15 min
  9. filtrationThe solid was filtered
  10. washwashed with ice cold water
  11. customdried

出典と根拠

ORDレコード
ord-1275a230bfbe4816ac5e531fb490dbae
出典データセット
uspto-grants-2012_03
特許番号
US08143237B2

反応ノート

読み込み中…