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Hydrochloric Acid → Spiro[indene-1,4'-piperidine] hydrochloride

HRID 1590627
ノート
印刷プレビュー

反応式

HRID 1590627 の反応式
C(OC([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)(C)(C)C.[ClH:22]>C(OCC)(=O)C>[ClH:22].[NH: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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 3653579Tert-butyl Spiro[indene-1,4'-piperidine]-1'-carboxylate

生成物 1

HCID 22509344Spiro[indene-1,4'-piperidine] hydrochloride

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

1'-(t-Butyloxycarbonyl)spiro(indene-1,4'-piperidine) (16 g, 56 mmole) in ethyl acetate (250 ml) was stirred in an ice bath and saturated with HCl(g) for 30 minutes. The mixture was evaporated to dryness. Ethyl acetate was added and removed in vacuo three times, and the residue was triturated with diethyl ether and filtered to provide spiro(1H-indene-1,4'-piperidine) hydrochloride. The free base was obtained by slurrying the hydrochloride in aqueous sodium bicarbonate solution and extracting with CH2Cl2. The organic layer was separated, dried over sodium sulfate, filtered, and evaporated to dryness in vacuo to provide spiro(1H-indene-1,4'piperidine.

後処理

  1. customThe mixture was evaporated to dryness
  2. additionEthyl acetate was added
  3. customremoved in vacuo three times
  4. customthe residue was triturated with diethyl ether
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-13b8684098b340cf8b77a7bf7d9e8827
出典データセット
uspto-grants-1993_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05204349

反応ノート

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