Iodine → HCID 178506566, 화합물

HRID 245784

반응식

HRID 245784 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[N:2]1.[I:10]I.[OH-].[K+]>CN(C=O)C>[I:10][C:3]1[C:4]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[NH:1][N:2]=1

참가 물질

5

반응물 3

HCID 807IodineHCID 92211H-IndazoleHCID 14797Potassium Hydroxide

생성물 1

HCID 178506566HCID 178506566, 화합물수율 99.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In a 50 mL round-bottomed flask, indazole (0.80 g, 6.8 mmol) was dissolved in DMF (14 mL). Iodine (3.4 g, 13.5 mmol) was added followed by potassium hydroxide (1.47 g, 26.2 mmol). The dark reaction mixture was stirred at room temperature for 1.25 h then was quenched with 10% aq NaHSO3 and extracted with diethyl ether (2×). The combined organic layers were washed with water and brine then dried over sodium sulfate, filtered and concentrated to give 1.65 g (95%) of 3-iodo-1H-indazole as a light yellow solid. 1H NMR (CDCl3, 300 MHz): δ (ppm) 10.56 (br. s, 1H), 7.47-7.57 (m, 3H), 7.23-7.30 (m, 1H).

후처리

  1. customThe dark reaction mixture
  2. customthen was quenched with 10% aq NaHSO3
  3. extractionextracted with diethyl ether (2×)
  4. washThe combined organic layers were washed with water and brine
  5. dry with materialthen dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-95d34199a9a34642b649aa1b6be2f693
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658646B2

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