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9-Borabicyclo(3.3.1)nonane → 1'-(t-butyloxycarbonyl)-3,4-dihydro-3-oxospiro[1H-indene-1,4'-piperidine]

HRID 266887
ノート
印刷プレビュー

反応式

HRID 266887 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11]2([C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[CH:14]2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].B1C2CCCC1CCC2.C1C=C[NH+]=CC=1.[O-:37][Cr](Cl)(=O)=O>C1COCC1.CCOCC>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][C:11]2([C:21]3[CH:16]([CH2:17][CH:18]=[CH:19][CH:20]=3)[C:15](=[O:37])[CH2:14]2)[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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

6

反応物 3

HCID 789669-Borabicyclo(3.3.1)nonaneHCID 3653579Tert-butyl Spiro[indene-1,4'-piperidine]-1'-carboxylateHCID 178418287HCID 178418287、化合物

生成物 1

HCID 190304391'-(t-butyloxycarbonyl)-3,4-dihydro-3-oxospiro[1H-indene-1,4'-piperidine]収率 47%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒
HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
70 °C

実験手順

To a solution of 661 mg (2.31 mmol) of 1'-(t-butyloxycarbonyl)spiro[1H-indene-1,4'-piperidine] [prepared by the method of Chambers, et al, J. Med. Chem., 1992, 35, 2036] in 5.0 ml of THF was added 5.8 ml (1.0M THF, 2.9 mmol) of 9-BBN. The reaction mixture was heated at 70° C. until TLC analysis indicated that the starting material was consumed. The solution was concentrated and the residue was dissolved in dichloromethane. The solution was cooled to 0° C. and 4.1 g (19.2 mmol) of PCC was added slowly over 15 minutes. The reaction mixture was warmed to room temperature and then to reflux for 30 minutes. The solution was then diluted with ether and filtered through a pad of a mixture of celite and florisil. Purification by flash chromotography (silica gel, hexane/ethyl acetate, 4:1) gave 326 mg (47%) of the title compound.

後処理

  1. customwas consumed
  2. concentrationThe solution was concentrated
  3. dissolutionthe residue was dissolved in dichloromethane
  4. temperatureThe solution was cooled to 0° C.
  5. temperatureThe reaction mixture was warmed to room temperature
  6. temperatureto reflux for 30 minutes
  7. filtrationfiltered through a pad of a mixture of celite and florisil
  8. customPurification by flash chromotography (silica gel, hexane/ethyl acetate, 4:1)

出典と根拠

ORDレコード
ord-261222eb6d5f4122b23c831fe8a56690
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05652235

反応ノート

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