Iodine → HCID 178477832, 화합물

HRID 245961

반응식

HRID 245961 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[NH:7][N:6]=[CH:5]2.[OH-].[K+].[I:14]I>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[NH:7][N:6]=[C:5]2[I:14]

참가 물질

5

반응물 3

HCID 807IodineHCID 14797Potassium HydroxideHCID 4123035,6-dichloro-1H-indazole

생성물 1

HCID 178477832HCID 178477832, 화합물수율 99%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 5,6-dichloro-1H-indazole (0.50 g, 2.67 mmol) in DMF (8 ml) at room temperature was added powdered potassium hydroxide (450 mg, 8.02 mmol) and iodine (1.02 g, 4.01 mmol). The maroon reaction mixture was stirred at room temperature for 45 min then quenched with 10% aqueous Na2S2O3 and diluted with water. The mixture was extracted with EtOAc (2×). The combined organics were washed with water (3×), dried over MgSO4 and concentrated to afford 827 mg (99%) of 5,6-dichloro-3-iodo-1H-indazole as a pale yellow solid. 1H NMR (DMSO-d6, 400 MHz): δ (ppm) 13.79 (s, 1H), 7.94 (s, 1H), 7.72 (s, 1H).

후처리

  1. customThe maroon reaction mixture
  2. customthen quenched with 10% aqueous Na2S2O3
  3. additiondiluted with water
  4. extractionThe mixture was extracted with EtOAc (2×)
  5. washThe combined organics were washed with water (3×)
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-091bfeade6204eedbc853379d096cb9f
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658646B2

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