Hydrochloric Acid → HCID 45263090、化合物

HRID 27246ノート

反応式

HRID 27246 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[CH2:23][CH2:22][C:21]2[C:16](=[C:17]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH:18]=[CH:19][CH:20]=2)[C:15]1=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[OH-].[Na+].[ClH:33]>CCOCC.O.O1CCCC1>[ClH:33].[CH2:7]([N:14]1[CH2:23][CH2:22][C:21]2[C:16](=[C:17]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH:18]=[CH:19][CH:20]=2)[CH2:15]1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 233443172-Benzyl-8-phenyl-3,4-dihydroisoquinolin-1(2H)-one

生成物 1

HCID 45263090HCID 45263090、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

3.6 Parts of lithium aluminum hydride is added to a solution of 10 parts of 2-benzyl-3,4-dihydro-8-phenyl-1(2H)-isoquinolone in 225 parts by volume dry tetrahydrofuran and the resulting mixture is stirred at reflux temperature for about 5 hours. Then the mixture is cooled in an ice bath and treated successively with 7.5 parts by volume of water in 15 parts by volume of tetrahydrofuran, 7.5 parts by volume of 25% sodium hydroxide, and 7.5 parts by volume of water. The salts which form are filtered off and the filtrate is dried over anhydrous magnesium sulfate and concentrated under reduced pressure to yield clear oil. The oil is taken up in ether and treated with isopropanolic hydrogen chloride to give, as a white solid, 2-benzyl-8-phenyl-1,2,3,4-tetrahydroisoquinoline hydrochloride, melting at about 187°-189° C. after recrystallization from a mixture of ethanol and ether. This compound has the following formula ##STR16##

後処理

  1. temperatureat reflux temperature for about 5 hours
  2. temperatureThen the mixture is cooled in an ice bath
  3. filtrationThe salts which form are filtered off
  4. dry with materialthe filtrate is dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto yield clear oil

出典と根拠

ORDレコード
ord-4ce3cf20126c41bb873dee78da9b6aa0
出典データセット
uspto-grants-1980_09
特許番号
US04220778

反応ノート

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