Ethylene Glycol → 1-(Pyrid-3-yl)-2-(2-bromophenyl)-ethanediol

HRID 1613639노트

반응식

HRID 1613639 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7](=[O:17])[CH:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[Br:16])O)[CH:2]=1.[BH4-].[Na+].Cl.C(O)C[OH:23]>CO>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([OH:17])([OH:23])[CH2:8][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[Br:16])[CH:2]=1

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 197741961-(Pyrid-3-yl)-2-(2-bromophenyl)-2-hydroxyethanone

생성물 1

HCID 197741971-(Pyrid-3-yl)-2-(2-bromophenyl)-ethanediol

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

20 g (0.068 mol) of 1-(pyrid-3-yl)-2-(2-bromophenyl)-2-hydroxyethanone in 300 ml of methanol were reduced with 3 g (0.079 mol) of sodium borohydride at 0° C. Stirring was carried out for a few hours at room temperature (21° C.), the pH was brought to 2 with 4N hydrochloric acid and 4 ml of ethylene glycol were added. The solution was evaporated down, after which the residue was covered with a layer of ethyl acetate and neutralized with NaHCO3 solution. The ethyl acetate phase was washed twice with water and dried over Na2SO4. After the ethyl acetate had been distilled off, the product was obtained as a white powder of melting point 115° C.

후처리

  1. waitwas carried out for a few hours at room temperature
  2. custom(21° C.)
  3. additionwere added
  4. customThe solution was evaporated down
  5. washThe ethyl acetate phase was washed twice with water
  6. dry with materialdried over Na2SO4
  7. distillationAfter the ethyl acetate had been distilled off
  8. customthe product was obtained as a white powder of melting point 115° C.

출처 및 근거

ORD 기록
ord-bcdbc5e5795b45fca221e53df83d02ea
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194441

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