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Bicyclo[2.2.2]octan-1-amine hydrochloride → 4-Aminobicyclo(2.2.2)octane

HRID 539606
ノート
印刷プレビュー

反応式

HRID 539606 の反応式
CC1(C)C(C)(C)OC(OC2C=CC([N+]([O-])=O)=CC=2)=NS1(=O)=O.Cl.[NH2:24][C:25]12[CH2:32][CH2:31][CH:28]([CH2:29][CH2:30]1)[CH2:27][CH2:26]2>ClCCl.C(N(CC)C(C)C)(C)C>[NH2:24][C:25]12[CH2:32][CH2:31][CH:28]([CH2:29][CH2:30]1)[CH2:27][CH2:26]2
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 2

HCID 13182386Bicyclo[2.2.2]octan-1-amine hydrochlorideHCID 718136815,5,6,6-Tetramethyl-2-(4-nitrophenoxy)-5,6-dihydro-1,4,3-oxathiazine 4,4-dioxide

生成物 1

HCID 5502144-Aminobicyclo(2.2.2)octane収率 131.5%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 81531Diisopropylethylamine溶媒

実験手順

300 mg of 5,5,6,6-tetramethyl-2-(4-nitrophenoxy)-5,6-dihydro-1,4,3-oxathiazine 4,4-dioxide and 163 mg of 1-aminobicyclo[2.2.2]octane hydrochloride were dissolved in a mixture of 5 ml of dichloromethane and 0.38 ml of N,N-diisopropylethylamine, and the mixture was stirred at room temperature for 72 hours. Subsequently, the reaction solution was concentrated by rotary evaporation and the residue was purified in a purification laboratory by means of preparative HPLC. After lyophilization of the product-containing fractions, the product (166 mg) was thus obtained with a molecular weight of 314.5 g/mol (C15H26N2O3S); MS (ESI): m/e=315 (M+H+).

後処理

  1. concentrationSubsequently, the reaction solution was concentrated by rotary evaporation
  2. customthe residue was purified in a purification laboratory by means of preparative HPLC

出典と根拠

ORDレコード
ord-082cb8e1755b4ea7809d1ee5dcab8bf9
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871758B2

反応ノート

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