Phosphorus oxychloride → HCID 60108780, 화합물

HRID 1296582노트

반응식

HRID 1296582 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11](O)([C:14]2[CH:15]=[CH:16][CH:17]=[C:18]3[C:22]=2[NH:21][CH:20]=[CH:19]3)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].P(Cl)(Cl)(Cl)=O>N1C=CC=CC=1>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH:10]=[C:11]([C:14]2[CH:15]=[CH:16][CH:17]=[C:18]3[C:22]=2[NH:21][CH:20]=[CH:19]3)[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 60108792HCID 60108792, 화합물

생성물 1

HCID 60108780HCID 60108780, 화합물수율 64%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

4-Hydroxy-4-(1-H-indol-7-yl)-piperidine-1-carboxylic acid tert-butyl ester XVI (1.17 g, 3.7 mmol) was combined with pyridine (20 mL) and phosphorus oxychloride (0.7 mL, 7.4 mmol) at room temperature under nitrogen, and was stirred overnight. The reaction was partitioned between ethyl acetate (55 mL) and water (55 mL). The ethyl acetate layer was washed with water (2×30 mL) and brine (55 mL), then dried (MgSO4), filtered and concentrated to afford (700 mg, 64%) of 4-(1H-indol-7-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester XVII.

후처리

  1. customThe reaction was partitioned between ethyl acetate (55 mL) and water (55 mL)
  2. washThe ethyl acetate layer was washed with water (2×30 mL) and brine (55 mL)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-63ecb31433234779858df98efec83f99
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07247651B2

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