Sodium Nitrite → HCID 136331513, 화합물

HRID 1097224노트

반응식

HRID 1097224 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 136331513HCID 136331513, 화합물수율 77%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

반응 조건

온도
0 °C

실험 절차

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)—.

후처리

  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

출처 및 근거

ORD 기록
ord-1275a230bfbe4816ac5e531fb490dbae
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143237B2

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