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Ammonium Chloride → HCID 86646304、化合物

HRID 1027136
ノート
印刷プレビュー

反応式

HRID 1027136 の反応式
[CH3:1][C:2]1(O)[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:4]2([CH2:9][CH2:8][N:7]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:6][CH2:5]2)[CH2:3]1.O.C1(C)C(S(O)(=O)=O)=CC=CC=1.[Cl-].[NH4+]>C(Cl)Cl>[CH3:1][C:2]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:4]2([CH2:9][CH2:8][N:7]([C:10]([O:12][C:13]([CH3:14])([CH3:15])[CH3:16])=[O:11])[CH2:6][CH2:5]2)[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 124969952-Methylbenzenesulfonic acid hydrateHCID 67082928tert-Butyl 1-methyl-1-hydroxyspiro[indane-3,4'-piperidine]-1'-carboxylate

生成物 1

HCID 86646304HCID 86646304、化合物収率 81.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

tert-Butyl 1-methyl-1-hydroxyspiro[indane-3,4′-piperidine]-1′-carboxylate (0.140 g, 0.441 mmol) obtained in step 1 was dissolved in methylene chloride (2 mL), toluenesulfonic acid monohydrate (0.008 g, 0.044 mmol) was added, and the mixture was stirred at room temperature for 3 hr. Saturated aqueous ammonium chloride solution was added dropwise to the reaction mixture, and the mixture was extracted several times with ethyl acetate. The combined organic layers were dried over magnesium sulfate and concentrated under reduced pressure to give the title compound (0.108 g, 81%).

後処理

  1. extractionthe mixture was extracted several times with ethyl acetate
  2. dry with materialThe combined organic layers were dried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2b84a62b41144231829142f49ac6e675
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08729264B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート