Dichloromethane → Ethyl 1-phenyl-3,4-dihydro-1H-isoquinoline-2-carboxylate

HRID 566372

反応式

HRID 566372 の反応式
ClCCl.[C:4]1([CH:10]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH2:13][CH2:12][NH:11]2)[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.Cl[C:21]([O:23][CH2:24][CH3:25])=[O:22]>C(N(CC)CC)C>[C:4]1([CH:10]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH2:13][CH2:12][N:11]2[C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 10928Ethyl chloroformateHCID 1001371,2,3,4-Tetrahydro-1-phenylisoquinoline

生成物 1

HCID 10423841Ethyl 1-phenyl-3,4-dihydro-1H-isoquinoline-2-carboxylate

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

To a 130 ml dichloromethane solution containing 6.28 g of 1-phenyl-1,2,3,4-tetrahydroisoquinoline and 3.34 g of triethylamine, 3.1 ml of ethyl chloroformate was added dropwise under ice-cooling, followed by stirring at room temperature overnight. The reaction solution was washed successively with water, 1N hydrochloric acid, water and brine and then dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, thereby 10.58 g of ethyl 1-phenyl-1,2,3,4-tetrahydro-2-isoquinolinecarboxylate was obtained as pale yellow oil.

後処理

  1. additionwas added dropwise under ice-
  2. temperaturecooling
  3. washThe reaction solution was washed successively with water, 1N hydrochloric acid, water and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-cb8ab4cd946e47f48cca1f6b54e680c7
出典データセット
uspto-grants-2001_01
特許番号
US06174896B1

関連ノート

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