Sodium borohydride → HCID 12953363, 화합물

HRID 355025노트

반응식

HRID 355025 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 12953363HCID 12953363, 화합물수율 7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1941379e11c04a5b873d59c3797bb92e
출처 데이터셋
uspto-grants-1983_03
특허 번호
US04377693

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