Phosphorus oxychloride → HCID 60108780、化合物

HRID 1296582ノート

反応式

HRID 1296582 の反応式
[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]

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 60108792HCID 60108792、化合物

生成物 1

HCID 60108780HCID 60108780、化合物収率 64%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-63ecb31433234779858df98efec83f99
出典データセット
uspto-grants-2007_07
特許番号
US07247651B2

反応ノート

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