Triethylamine → HCID 10760500, 화합물

HRID 1637383노트

반응식

HRID 1637383 반응식
C(N(CC)CC)C.[CH3:8][S:9]([N:12]([CH3:18])[NH:13][S:14]([CH3:17])(=[O:16])=[O:15])(=[O:11])=[O:10].Cl[C:20]([O:22][CH2:23][CH2:24][Br:25])=[O:21]>CC(C)=O>[CH3:8][S:9]([N:12]([CH3:18])[N:13]([S:14]([CH3:17])(=[O:15])=[O:16])[C:20]([O:22][CH2:23][CH2:24][Br:25])=[O:21])(=[O:10])=[O:11]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 785282-Bromoethyl chloroformateHCID 1306301,2-Bis(methylsulfonyl)-1-methylhydrazine

생성물 1

HCID 10760500HCID 10760500, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

1,2-Bis(methylsulfonyl)-2-(2-bromoethoxycarbonyl)-1-methylhydrazine (compound 8) was synthesized as follows: Triethylamine (1.45 g, 0.014 mol) was added in portions to a stirred solution of 1,2-bis(methylsulfonyl)-1-methylhydrazine (2.02 g, 0.01 mol) and 2-bromoethyl chloroformate (3.49 g, 0.019 mol) in acetone (100 ml) over a period of 15 min. The reaction mixture was stirred for an additional 18 hr, filtered, and the filtrate evaporated to dryness in vacuo. The residue was taken up in chloroform (100 ml) and washed with water (3×20 ml). The chloroform layer was dried over anhydrous magnesium sulfate, filtered, and the filtrate evaporated to dryness. The residue was triturated with petroleum ether until a solid separated. The solid was filtered and recrystallized from ethanol (1.52 g, 43.0%). Mp was approximately 81-82° C. 1H NMR (CDCl3): δ 4.7 and 3.6 (4H, 2t, CH2CH2Br), 3.5, 3.3 and 3.1 (9H, 3s, 2CH3SO2 and NCH3).

후처리

  1. filtrationfiltered
  2. customthe filtrate evaporated to dryness in vacuo
  3. washwashed with water (3×20 ml)
  4. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customthe filtrate evaporated to dryness
  7. customThe residue was triturated with petroleum ether until a solid
  8. customseparated
  9. filtrationThe solid was filtered
  10. customrecrystallized from ethanol (1.52 g, 43.0%)

출처 및 근거

ORD 기록
ord-ca28403d03ad4a80b3c5eb01499c9e98
출처 데이터셋
uspto-grants-2000_03
특허 번호
US06040338

반응 노트

불러오는 중…