Sodium Iodide → HCID 67313226、化合物

HRID 222062ノート

反応式

HRID 222062 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[CH:5]=[CH:4][C:3]=1[OH:11].Cl.Cl[CH2:14][C:15]1[N:16]=[CH:17][S:18][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>C(#N)C.C(Cl)Cl.O>[ClH:1].[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[O:11][CH2:14][C:15]1[N:16]=[CH:17][S:18][CH:19]=1

参加物

8

反応物 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 12074NitrofunginHCID 27632894-(Chloromethyl)-1,3-thiazole hydrochloride

生成物 1

HCID 67313226HCID 67313226、化合物収率 83%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-chloro-4-nitrophenol (1.00 g, 5.76 mmol) in acetonitrile (125 mL) were added 4-chloromethylthiazole hydrochloride (1.08 g, 6.34 mmol), Potassium carbonate (2.39 g, 17.29 mmol) and sodium iodide (1.73 g, 11.52 mmol). The reaction mixture was stirred at 60 C overnight. Water (60 mL) and DCM (10 mL) were added. After all solid material dissolved, layers formed were separated. The organic layer was washed with water and brine, dried over Na2SO4 and concentrated down to give the required material as a light yellow solid (1.29 mg, 83%). 1H-NMR (CD2Cl2) δ 8.87 (d, 1H), 8.32 (d, 1H), 8.16 (dd, 1H), 7.54-7.56 (m, 1H), 7.22 (d, 1H), 5.33-5.34 (m, 2H); LCMS RT=3.01 min; [M+H]+=271.0.

後処理

  1. dissolutionAfter all solid material dissolved
  2. customlayers formed
  3. customwere separated
  4. washThe organic layer was washed with water and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated down

出典と根拠

ORDレコード
ord-407926c603784d78906a5cde6a1da983
出典データセット
uspto-grants-2012_06
特許番号
US08207172B2

反応ノート

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