Sodium borohydride → HCID 67369877、化合物

HRID 383985ノート

反応式

HRID 383985 の反応式
[BH4-].[Na+].[F:3][C:4]1[CH:13]=[C:12]2[C:7]([CH2:8][CH2:9][N:10]=[C:11]2[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:6][CH:5]=1>CCO>[F:3][C:4]1[CH:13]=[C:12]2[C:7]([CH2:8][CH2:9][NH:10][CH:11]2[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)=[CH:6][CH:5]=1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 67367547HCID 67367547、化合物

生成物 1

HCID 67369877HCID 67369877、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.65 g (17.1 mmol) of NaBH4 were added in portions to a solution of 3.2 g (max. 14.2 mmol) of the crude product 7-fluoro-1-phenyl-3,4-dihydroisoquinoline in EtOH (80 ml) and the mixture was then stirred for 16 h at RT. Then the mixture was concentrated to small volume under vacuum and the residue was taken up with DCM (200 ml). It was washed with water and the aqueous phase was extracted with DCM (2×150 ml). The combined organic phases were washed with brine, dried over Na2SO4, filtered and concentrated to small volume under vacuum. 7-Fluoro-1-phenyl-1,2,3,4-tetrahydroisoquinoline was obtained as the crude product, which was reacted further with no additional purification.

後処理

  1. concentrationThen the mixture was concentrated to small volume under vacuum
  2. washIt was washed with water
  3. extractionthe aqueous phase was extracted with DCM (2×150 ml)
  4. washThe combined organic phases were washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated to small volume under vacuum

出典と根拠

ORDレコード
ord-4138668e6cef4e1d9b10c6c7ce60c519
出典データセット
uspto-grants-2013_02
特許番号
US08367700B2

反応ノート

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