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Hydrochloric Acid → 3-Bromo-2-methylaminomethyl-phenylamine

HRID 459790
ノート
印刷プレビュー

反応式

HRID 459790 の反応式
C(O[C:6](=O)[N:7]([CH2:9][C:10]1[C:15]([Br:16])=[CH:14][CH:13]=[CH:12][C:11]=1[NH2:17])C)(C)(C)C.Cl.C([O-])(O)=O.[Na+].C(OCC)(=O)C>C(O)C>[Br:16][C:15]1[C:10]([CH2:9][NH:7][CH3:6])=[C:11]([NH2:17])[CH:12]=[CH:13][CH:14]=1
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 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 58824133(2-Amino-6-bromo-benzyl)-methyl-carbamic acid tert-butyl ester

生成物 1

HCID 184444723-Bromo-2-methylaminomethyl-phenylamine収率 765.5%

試薬・触媒・溶媒 1

HCID 702Ethanol
溶媒

反応条件

温度
100 °C

実験手順

(2-Amino-6-bromo-benzyl)-methyl-carbamic acid tert-butyl ester (371 mg) was dissolved in 50 ml ethanol. To this solution was added 2M ethanolic hydrochloride acid solution (10 ml). The reaction mixture was heated at 100° C. for 30 minutes, at which time the deprotection was completed. The solution was allowed to cool to room temperature and poured into the mixture of saturated NaHCO3 solution and ethyl acetate. The aqueous layer was extracted with EtOAc three times and the organic fractions were concentrated to give 3-bromo-2-methylaminomethyl-phenylamine as a brown oil (1.938 g, 76%). MS: (M+H)+217.1.

後処理

  1. temperatureto cool to room temperature
  2. extractionThe aqueous layer was extracted with EtOAc three times
  3. concentrationthe organic fractions were concentrated

出典と根拠

ORDレコード
ord-47f0bde3834a410da7b8f1065629cbe4
出典データセット
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07196087B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート