Triethylamine → HCID 10760500、化合物

HRID 1637383ノート

反応式

HRID 1637383 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 10760500HCID 10760500、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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).

後処理

  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%)

出典と根拠

ORDレコード
ord-ca28403d03ad4a80b3c5eb01499c9e98
出典データセット
uspto-grants-2000_03
特許番号
US06040338

反応ノート

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