Sodium Iodide → HCID 35155、化合物

HRID 1533468ノート

反応式

HRID 1533468 の反応式
[Br:1][CH:2]([Br:15])[C:3]1[N:8]=[C:7]([CH:9](Br)Br)[N:6]=[C:5]([CH:12]([Br:14])[Br:13])[N:4]=1.[I-].[Na+].S(=O)(O)[O-].[Na+]>CC(C)=O.C(O)(=O)C>[Br:14][CH:12]([Br:13])[C:5]1[N:4]=[C:3]([CH:2]([Br:1])[Br:15])[N:8]=[C:7]([CH3:9])[N:6]=1

参加物

6

反応物 3

HCID 5238Sodium IodideHCID 351561,3,5-Triazine, 2,4,6-tris(dibromomethyl)-HCID 23665763Sodium Bisulfite

生成物 1

HCID 35155HCID 35155、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 180Acetone溶媒2 回

実験手順

A solution of 2,4,6-tris(dibromomethyl)-s-triazine (15 g, 23.3 mmol) in acetone (100 mL) was added to a solution of sodium iodide (150 g, 1.0 mol) in acetic acid (50 mL) and acetone (500 mL). After 10 minutes at room temperature the reaction mixture was added to sodium bisulfite (25 g) in ice water (1000 mL). The aqueous layer was extracted with ether (3×100 mL). The ether layer was dried (MgSo4), filtered, and concentrated to dryness. The crude product was crystallized first from EtOH and then from cyclohexane to give the title compound (mp 87-88.5° C.). 1H NMR (CDCL3) δ2.51 (s, 3H, CH3), 6.86 (s, 2H, CH).

後処理

  1. extractionThe aqueous layer was extracted with ether (3×100 mL)
  2. dry with materialThe ether layer was dried (MgSo4)
  3. filtrationfiltered
  4. concentrationconcentrated to dryness
  5. customThe crude product was crystallized first from EtOH

出典と根拠

ORDレコード
ord-2487a7c30fe34b199a2f28e122f7d33f
出典データセット
uspto-grants-2001_03
特許番号
US06207826B1

反応ノート

読み込み中…