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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 21993816、化合物

HRID 1978336
ノート
印刷プレビュー

反応式

HRID 1978336 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([CH:13]2[CH2:18][CH2:17][N:16]([CH:19]3[CH2:24][CH2:23][CH:22]([C:25](OC)=[O:26])[CH2:21][CH2:20]3)[CH2:15][CH2:14]2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(OCC)(=O)C.O>O1CCCC1>[C:7]1([CH:13]2[CH2:14][CH2:15][N:16]([CH:19]3[CH2:24][CH2:23][CH:22]([CH2:25][OH:26])[CH2:21][CH2:20]3)[CH2:17][CH2:18]2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 21226445Aluminium lithium hydride2 回HCID 21993968HCID 21993968、化合物

生成物 1

HCID 21993816HCID 21993816、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of 0.36 g (9.37 mM) of lithium aluminum hydride in 50 ml of tetrahydrofuran was added a solution of 2.825 g (9.372 mM) of methyl 4-(4-phenylpiperidino)cyclohexanecarboxylate in 50 ml of tetrahydrofuran dropwise with ice-cooling and the mixture was stirred at room temperature for one hour. To this reaction mixture was added ethyl acetate with ice-cooling to decompose the excess lithium aluminum hydride. Then, water was added until a white precipitate had formed. The precipitate was filtered off with the aid of celite and washed with ethyl acetate. The filtrate and washes were pooled and the solvent was distilled off under reduced pressure. The solid residue was rinsed with diethyl ether-hexane to provide the title compound.

後処理

  1. temperaturecooling
  2. temperaturecooling
  3. customhad formed
  4. filtrationThe precipitate was filtered off with the aid of celite
  5. washwashed with ethyl acetate
  6. distillationthe solvent was distilled off under reduced pressure
  7. washThe solid residue was rinsed with diethyl ether-hexane

出典と根拠

ORDレコード
ord-db94d560ff9c471a94c1c2901cb3167b
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06235731B1

反応ノート

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