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Hydrochloric Acid → 2-Butyl-3-oxo-1,2,3,4,5,6,7,8-octahydroisoquinoline-4-carbonitrile

HRID 1994276
ノート
印刷プレビュー

反応式

HRID 1994276 の反応式
[CH2:1]([N:5]1[C:14](=[O:15])[C:13]([C:16]#[N:17])=[C:12]2[C:7]([CH2:8][CH2:9][CH2:10][CH2:11]2)=[CH:6]1)[CH2:2][CH2:3][CH3:4].C1(C)C=CC=CC=1.[H-].C([Al+]CC(C)C)C(C)C.Cl>C1(C)C=CC=CC=1>[CH2:1]([N:5]1[C:14](=[O:15])[CH:13]([C:16]#[N:17])[C:12]2[CH2:11][CH2:10][CH2:9][CH2:8][C:7]=2[CH2:6]1)[CH2:2][CH2:3][CH3:4]
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 3

HCID 313Hydrochloric AcidHCID 222664592-Butyl-3-oxo-2,3,5,6,7,8-hexahydroisoquinoline-4-carbonitrileHCID 86583787Diisobutylaluminumhydride toluene

生成物 1

HCID 222665342-Butyl-3-oxo-1,2,3,4,5,6,7,8-octahydroisoquinoline-4-carbonitrile収率 70.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

2-Butyl-3-oxol-2,3,5,6,7,8-hexahydroisoquinoline-4-carbonitrile (7-012) (100 mg, 0.43 mmol) was dissolved in toluene (10 mL), and to the reaction mixture was added 1 M diisobutylaluminium hydride toluene solution (0.8 mL, 0.8 mmol) under ice-cooling, and the reaction mixture was stirred for 10 min. To the reaction mixture was added 1 mol/L diluted hydrochloric acid (5 mL), and the reaction mixture was extracted with ethyl acetate (10 mL), washed with brine (5 mL), dried over anhydrous magnesium sulfate, and evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (toluene/ethyl acetate) to give 2-butyl-3-oxo-1,2,3,4,5,6,7,8-octahydroisoquinoline-4-carbonitrile (7-018) (70 mg, 70%) as a white powder.

後処理

  1. temperaturecooling
  2. extractionthe reaction mixture was extracted with ethyl acetate (10 mL)
  3. washwashed with brine (5 mL)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography (toluene/ethyl acetate)

出典と根拠

ORDレコード
ord-f65e8d561c3b4a07ac15ec2ef79d2c68
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07652141B2

反応ノート

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