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Tetrahydrofuran → HCID 59865005、化合物

HRID 1669743
ノート
印刷プレビュー

反応式

HRID 1669743 の反応式
I[C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][CH2:15][C:14]([CH3:19])([CH3:18])[CH2:13]2)=[CH:4][CH:3]=1.C([Mg]Cl)(C)C.[C:25]([N:32]1[CH2:37][CH2:36][CH2:35][CH2:34][C:33]1=O)([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26].[Cl-].[NH4+].C1C[O:44]CC1>C(OCC)(=O)C>[CH3:18][C:14]1([CH3:19])[CH2:15][CH2:16][CH2:17][N:12]([CH2:11][CH2:10][CH2:9][O:8][C:5]2[CH:6]=[CH:7][C:2]([C:35]3([OH:44])[CH2:36][CH2:37][N:32]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:33][CH2:34]3)=[CH:3][CH:4]=2)[CH2:13]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 8028Tetrahydrofuran2 回HCID 25517Ammonium ChlorideHCID 7577838tert-Butyl 2-oxopiperidine-1-carboxylateHCID 59865001HCID 59865001、化合物HCID 178418918HCID 178418918、化合物

生成物 1

HCID 59865005HCID 59865005、化合物

試薬・触媒・溶媒 1

HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
2.5 °C

実験手順

A solution of 1-{3-[(4-iodophenyl)oxy]propyl}-3,3-dimethylpiperidine (25 g) in THF (125 ml) is stirred for about 15 min, then cooled to 0-5° C. Isopropyl magnesium chloride solution (70.5 ml, 1.9M) is added at 0-5° C. over about 40 min, then the mixture is stirred at 0-5° C. for 2-3 h. The mixture is then cooled to −78 to −80° C. and a precooled solution (−20 to −30° C.) of N-Boc-piperidinone (16 g) in THF (125 ml) is added over about 1-2 h and the reaction mixture is stirred for about 1.5 h at −78 to −80° C. The reaction mixture is allowed to warm to 25-30° C., then stirred for 23-24 h. Saturated ammonium chloride solution (375 ml) is added at 25-30° C., followed by ethyl acetate (500 ml) and the mixture stirred for about 50 min. The aqueous layer is extracted with ethyl acetate (250 ml). The combined organic layers are washed with water (375 ml), dried over sodium sulfate and concentrated under reduced pressure to give the crude title compound (30.3 g).

後処理

  1. temperatureThe mixture is then cooled to −78 to −80° C.
  2. stirringthe reaction mixture is stirred for about 1.5 h at −78 to −80° C
  3. temperatureto warm to 25-30° C.
  4. stirringstirred for 23-24 h
  5. stirringthe mixture stirred for about 50 min
  6. extractionThe aqueous layer is extracted with ethyl acetate (250 ml)
  7. washThe combined organic layers are washed with water (375 ml)
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-50fc68c6c393496ea348f08e7362dd7d
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07989629B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート