Lithium borohydride → HCID 18779681、化合物

HRID 1421762ノート

反応式

HRID 1421762 の反応式
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([C:10]#[N:11])=[C:6]([C:12]#[N:13])[CH:5]=1.[Li+].[BH4-]>C1COCC1>[OH:2][CH2:3][C:4]1[CH:5]=[C:6]([C:12]#[N:13])[C:7](=[CH:8][CH:9]=1)[C:10]#[N:11]

参加物

4

反応物 2

HCID 4148881Lithium borohydrideHCID 14495336HCID 14495336、化合物

生成物 1

HCID 18779681HCID 18779681、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
70 °C

実験手順

3,4-Dicyano-benzoic acid methyl ester from step 1 (2.4 g, 12.9 mmol ) was dissolved in THF (65 ml). LiBH4 in THF (2 M, 12.9 ml, 25.8 mmol) was added. The reaction mixture was heated to 70° C. for 3 hours. The reaction was quenched carefully with 3N HCl and then extracted with EtOAc (3×20 mL). The organic layers were combined, washed with brine, dried (MgSO4), filtered and concentrated to yield the desired product.

後処理

  1. customThe reaction was quenched carefully with 3N HCl
  2. extractionextracted with EtOAc (3×20 mL)
  3. washwashed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-d0684c9bc57c46819bd5b608c81902ac
出典データセット
uspto-grants-2000_06
特許番号
US06077853

反応ノート

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