Dimethylamine → n,n-dimethyl-1,2,3,4-tetrahydronaphthalen-2-amine

HRID 2088738ノート

反応式

HRID 2088738 の反応式
CO.CN(C)C[CH:6]1[CH2:15][CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1.[CH3:17][NH:18][CH3:19].C1C(=O)CC2C(=CC=CC=2)C1>O1CCCC1>[CH3:17][N:18]([CH3:19])[CH:6]1[CH2:15][CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1

参加物

6

反応物 4

HCID 674DimethylamineHCID 887MethanolHCID 682662-TetraloneHCID 21063044HCID 21063044、化合物

生成物 1

HCID 242461n,n-dimethyl-1,2,3,4-tetrahydronaphthalen-2-amine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

46 ml of a methanol solution of 0.3 M sodium cyanoborohydride-1/2 zinc chloride and 6.9 mL of a tetrahydrofuran solution of 2 M dimethylamine were added to a tetrahydrofuran (10 mL) solution of 2.02 g of β-tetralone, and stirred for a day at room temperature. The reaction liquid was concentrated, and 1 N hydrochloric acid was added thereto. The acidic solution was washed with ethyl acetate, then made alkaline with aqueous 5 M sodium hydroxide solution, and extracted with ethyl acetate. This was washed with saturated saline water, dried with anhydrous magnesium sulfate, and the solvent was evaporated away to obtain 857 mg of the entitled compound as a colorless oily substance.

後処理

  1. customThe reaction liquid
  2. concentrationwas concentrated
  3. addition1 N hydrochloric acid was added
  4. washThe acidic solution was washed with ethyl acetate
  5. extractionextracted with ethyl acetate
  6. washThis was washed with saturated saline water
  7. dry with materialdried with anhydrous magnesium sulfate
  8. customthe solvent was evaporated away

出典と根拠

ORDレコード
ord-6196f24260f544bb88b4ad4091c8b7d6
出典データセット
uspto-grants-2013_05
特許番号
US08436004B2

反応ノート

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