Boron tribromide → HCID 11638630、化合物

HRID 19969ノート

反応式

HRID 19969 の反応式
C[O:2][C:3]1[CH:4]=[C:5]([NH:14][C:15](=[O:25])[C:16]2[CH:21]=[CH:20][C:19]3[O:22]C[O:24][C:18]=3[CH:17]=2)[CH:6]=[CH:7][C:8]=1[NH:9][S:10]([CH3:13])(=[O:12])=[O:11].B(Br)(Br)Br>CO>[OH:2][C:3]1[CH:4]=[C:5]([NH:14][C:15](=[O:25])[C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[C:18]([OH:24])[CH:17]=2)[CH:6]=[CH:7][C:8]=1[NH:9][S:10]([CH3:13])(=[O:12])=[O:11]

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 37259044N-(3-methoxy-4-methanesulfonylaminophenyl)-3,4-methylenedioxybenzamide

生成物 1

HCID 11638630HCID 11638630、化合物収率 33.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred suspension of N-(3-methoxy-4-methanesulfonylaminophenyl)-3,4-methylenedioxybenzamide (200 mg) in dry CH3Cl2 (20 ml) under nitrogen, was added boron tribromide (0.3 ml) then stirring continued for a further 20 hours. Methanol (50 ml) was added carefully, then the solvent evaporated in vacuo to a volume of 1 ml, this was repeated 2 more times. Purification by column chromatography over silica gel eluting with chloroform containing methanol (10-20%) gave N-(3-hydroxy-4-methanesulfonylaminophenyl)-3,4-dihydroxybenzamide (62 mg, 33%) as pale brown crystals.

後処理

  1. customthe solvent evaporated in vacuo to a volume of 1 ml
  2. customPurification by column chromatography over silica gel eluting with chloroform
  3. additioncontaining methanol (10-20%)

出典と根拠

ORDレコード
ord-bab2e04925e64859980f622da98ae4e7
出典データセット
uspto-grants-2010_06
特許番号
US07745490B2

反応ノート

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