Boron tribromide → HCID 21706255、化合物

HRID 1594922ノート

反応式

HRID 1594922 の反応式
B(Br)(Br)Br.[CH3:5][C:6]1([CH:14]2[NH:20][C:19](=[O:21])[CH2:18][CH2:17][CH2:16][CH2:15]2)[CH:11]=[CH:10][CH:9]=[C:8]([O:12]C)[CH2:7]1>C(Cl)(Cl)Cl>[CH3:5][C:6]1([CH:14]2[NH:20][C:19](=[O:21])[CH2:18][CH2:17][CH2:16][CH2:15]2)[CH:11]=[CH:10][CH:9]=[C:8]([OH:12])[CH2:7]1

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 21706269HCID 21706269、化合物

生成物 1

HCID 21706255HCID 21706255、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

BBr3 (1M in CH2Cl2) (1 mL, 1 mmol) was added dropwise to a solution of 7-(1-methyl-3-methoxyphenyl)-azepan-2-one, as described in Step D above, (0.06 g, 0.26 mmol) in CHCl3 (1 mL) at 0° C. with stirring. The ice bath was removed and stirring was continued for 1 h. The reaction mixture was partitioned between EtOAc (100 mL)—H2O (100 mL), the organic layer separated, washed with H2O, dried (MgSO4), filtered and concentrated to give the title compound after SiO2 chromatography (CHCl3:MeOH, 10:1).

後処理

  1. customat 0° C.
  2. customThe ice bath was removed
  3. stirringstirring
  4. customThe reaction mixture was partitioned between EtOAc (100 mL)—H2O (100 mL)
  5. customthe organic layer separated
  6. washwashed with H2O
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-ba9941c0c4ea4de9add891c79c61b6a5
出典データセット
uspto-grants-2001_09
特許番号
US06284755B1

反応ノート

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