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Chlorosuccinimide → HCID 67165350, 화합물

HRID 552221
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HRID 552221 반응식
[CH3:1][C:2]1[C:14]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[NH:7][C:6]=2[CH:5]=[N:4][CH:3]=1.C1C(=O)N([Cl:22])C(=O)C1.C(=O)(O)[O-].[Na+]>Cl>[Cl:22][C:11]1[CH:12]=[C:13]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6]1[CH:5]=[N:4][CH:3]=[C:2]([CH3:1])[C:14]2=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 31398ChlorosuccinimideHCID 516892Sodium BicarbonateHCID 593375704-Methyl-9H-beta-carboline

생성물 1

HCID 67165350HCID 67165350, 화합물수율 93.7%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

4-methyl-9H-β-carboline (97 mg, 0.532 mmol) was dissolved in HCl (1N, 4 ml) and stirred at RT. NCS (85 mg, 0.637 mmol) was added thereto and the reaction mixture was stirred for 5 hr. Saturated sodium bicarbonate solution (20 ml) was added thereto and the reaction mixture was extracted twice with EtOAc (100 ml). The combined organic layers were washed with brine, dried over MgSO4, filtered, and concentrated to give 6-chloro-4-methyl-9H-β-carboline (108 mg) as an oil. 1H-NMR (300 MHz, DMSO-d6): δ 8.67 (s, 1); 8.19 (s, 1); 8.11 (s, 1); 7.57-7.54 (m, 2); 2.82 (s, 3). NH4OAc standard conditions. DAD Rf=2.48 min. M+H=217.

후처리

  1. stirringthe reaction mixture was stirred for 5 hr
  2. extractionthe reaction mixture was extracted twice with EtOAc (100 ml)
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2f34d6c6f4414743b69ce1c5114d9ff5
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07951801B2

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