Potassium Carbonate → HCID 68465364, 화합물

HRID 501176

반응식

HRID 501176 반응식
[CH3:1][O:2][C:3](=[O:11])[C:4]1[CH:9]=[CH:8][C:7](Cl)=[N:6][CH:5]=1.[CH2:12]1[C:17]2[NH:18][C:19]3[C:24]([C:16]=2[CH2:15][CH2:14][NH:13]1)=[CH:23][CH:22]=[CH:21][CH:20]=3.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1>[CH2:12]1[C:17]2[NH:18][C:19]3[C:24](=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:16]=2[CH2:15][CH2:14][N:13]1[C:7]1[CH:8]=[CH:9][C:4]([C:3]([O:2][CH3:1])=[O:11])=[CH:5][N:6]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 107838Tetrahydro-beta-carboline2회HCID 254249Methyl 6-chloropyridine-3-carboxylate

생성물 1

HCID 68465364HCID 68465364, 화합물수율 24.7%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
100 °C

실험 절차

A mixture of methyl-6-chloronicotinate (170 mg), 1,2,3,4-tetrahydro-9H-pyrido[3,4-b]indole (170 mg), potassium carbonate (150 mg) and dioxane (6 mL) was heated in a 100° C. oil bath overnight. Another aliquote of 1,2,3,4-tetrahydro-9H-pyrido[3,4-b]indole (170 mg) was added and the heating was continue for five hours. The reaction was cooled and partitioned between water and EtOAc. The organics were washed with water, dried, and the solvent evaporated. The residue was purified by filtration through silica gel eluting with EtOAc to give methyl 6-(1,3,4,9-tetrahydro-2H-b-carbolin-2-yl)nicotinate as a brown solid (75 mg), m/e=308 (M+1).

후처리

  1. temperatureThe reaction was cooled
  2. custompartitioned between water and EtOAc
  3. washThe organics were washed with water
  4. customdried
  5. customthe solvent evaporated
  6. filtrationThe residue was purified by filtration through silica gel eluting with EtOAc

출처 및 근거

ORD 기록
ord-e40b2c5d20dd461a9df9ecd20adfc17b
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772245B2

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