Sodium borohydride → HCID 12953363、化合物

HRID 355025ノート

反応式

HRID 355025 の反応式
[Cl:1][C:2]1[S:3][C:4]([C:14](OCC)=[O:15])=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=2)[N:6]=1.[BH4-].[Na+]>C(O)C>[Cl:1][C:2]1[S:3][C:4]([CH2:14][OH:15])=[C:5]([C:7]2[CH:8]=[CH:9][C:10]([Cl:13])=[CH:11][CH:12]=2)[N:6]=1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 13041832Ethyl 2-chloro-4-(p-chlorophenyl)-5-thiazolecarboxylate

生成物 1

HCID 12953363HCID 12953363、化合物収率 7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of 18.2 g (0.06 mol) of ethyl 2-chloro-4-(p-chlorophenyl)-5-thiazolecarboxylate in 100 ml of ethanol was added 2.27 g (0.06 mol) of sodium borohydride. The reaction mixture was stirred for 1 hour and filtered. The ethanol filtrate was concentrated under reduced pressure and the residue was treated with water and extracted with CHCl3. The CHCl3 extracts were dried over MgSO4 and concentrated under reduced pressure. The residual solid (1.5 g) was recrystallized from ethanol-water to give 1.1 g (6%) of 2-chloro-4-(p-chlorophenyl)-5-thiazolemethanol, mp 113°-114° C.

後処理

  1. filtrationfiltered
  2. concentrationThe ethanol filtrate was concentrated under reduced pressure
  3. additionthe residue was treated with water
  4. extractionextracted with CHCl3
  5. dry with materialThe CHCl3 extracts were dried over MgSO4
  6. concentrationconcentrated under reduced pressure
  7. customThe residual solid (1.5 g) was recrystallized from ethanol-water

出典と根拠

ORDレコード
ord-1941379e11c04a5b873d59c3797bb92e
出典データセット
uspto-grants-1983_03
特許番号
US04377693

反応ノート

読み込み中…