Methanol → HCID 178508149、化合物

HRID 2218971ノート

反応式

HRID 2218971 の反応式
[C:1]1([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:6]=[CH:5][C:4]([NH2:7])=[C:3]([NH2:8])[CH:2]=1.CO.O.[N:18]#[C:19]Br>C1COCC1>[C:9]1([C:1]2[CH:6]=[CH:5][C:4]3[NH:7][C:19]([NH2:18])=[N:8][C:3]=3[CH:2]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

参加物

6

反応物 4

HCID 887MethanolHCID 962WaterHCID 10476Cyanogen BromideHCID 6452000(1,1'-Biphenyl)-3,4-diamine

生成物 1

HCID 178508149HCID 178508149、化合物収率 71%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of biphenyl-3,4-diamine (0.99 mmol) in THF:MeOH:water (5 mL:10 mL:10 mL) was added cyanogen bromide (5M solution in acetonitrile, 1.06 mmol). The resulting mixture was stirred at room temperature overnight. The reaction was partitioned between EtOAc and aqueous sodium hydroxide and the aqueous layer re-extracted with EtOAc. The combined EtOAc extracts were washed with water, brine, dried over MgSO2, then concentrated in vacuo to afford 7 (147 mg, 71%) as an off-white solid.

後処理

  1. customThe reaction was partitioned between EtOAc and aqueous sodium hydroxide
  2. extractionthe aqueous layer re-extracted with EtOAc
  3. washThe combined EtOAc extracts were washed with water, brine
  4. dry with materialdried over MgSO2
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e4d567a74cd846cb8054652dbd491677
出典データセット
uspto-grants-2008_08
特許番号
US07414046B2

反応ノート

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