Tetrahydrofuran → HCID 18779765、化合物

HRID 1421758ノート

反応式

HRID 1421758 の反応式
ClC1C=CC(=O)N(C2C=CC(CC3N([CH2:20][C:21]4[CH:26]=[C:25]([C:27]5[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=5)[C:24]([C:33]#[N:34])=[CH:23][CH:22]=4)C=NC=3)=CN=2)C=1.[Li+].[BH4-].C1C[O:41]CC1>>[OH:41][CH2:20][C:21]1[CH:26]=[C:25]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:24]([C:33]#[N:34])=[CH:23][CH:22]=1

参加物

4

反応物 3

HCID 8028Tetrahydrofuran2 回HCID 4148881Lithium borohydrideHCID 18779714HCID 18779714、化合物

生成物 1

HCID 18779765HCID 18779765、化合物

反応条件

温度
70 °C

実験手順

6-Cyano-biphenyl-3-carboxylic acid methyl ester from step 2 (1.4 g, 5.9 mmol) was dissolved in THF (24 ml). LiBH4 in THF (2 M, 5.9 ml, 11.8 mmol) was added. The reaction mixture was heated to 70° C. for 3 hours. The reaction mixture 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 mixture 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-fcd2af2ec02e4bf5b3aea99cfb3d5916
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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