N-Iodosuccinimide → HCID 178522276, 화합물

HRID 2283472노트

반응식

HRID 2283472 반응식
[OH:1][C:2]1[C:7]([NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:6][CH:5]=[CH:4][N:3]=1.C1C(=O)N([I:26])C(=O)C1>C(Cl)Cl>[OH:1][C:2]1[C:7]([NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)=[CH:6][C:5]([I:26])=[CH:4][N:3]=1

참가 물질

4

반응물 2

HCID 120273N-IodosuccinimideHCID 178522213HCID 178522213, 화합물

생성물 1

HCID 178522276HCID 178522276, 화합물수율 65.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of benzyl (2-hydroxypyridin-3-yl)carbamate (16.1 g, 65.9 mmol) in DCM (500 mL) was added NIS (17.8 g, 79.1 mmol) and the mixture heated at reflux overnight. After cooling, the mixture was filtered to afford benzyl (2-hydroxy-5-iodopyridin-3-yl)carbamate (16 g, 65% yield) as a white solid: 1H NMR (400 MHz, CDCl3) δ 8.27 (s, 1H), 7.72 (s, 1H), 7.29-7.40 (m, 5H), 5.21 (s, 2H); MS (ES) m/z 370 (M+H).

후처리

  1. temperaturethe mixture heated
  2. temperatureat reflux overnight
  3. temperatureAfter cooling
  4. filtrationthe mixture was filtered

출처 및 근거

ORD 기록
ord-bc1ecfc34a0b4e7eb537f3f5c8ab71d7
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09145393B2

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