Sodium Iodide → HCID 35155, 화합물

HRID 1533468노트

반응식

HRID 1533468 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 35155HCID 35155, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 180Acetone용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-2487a7c30fe34b199a2f28e122f7d33f
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06207826B1

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