Acetic Acid → HCID 70396304, 화합물

HRID 1723097

반응식

HRID 1723097 반응식
[CH2:1]([N:3]([C:8]1[CH:13]=[CH:12][C:11]([CH:14]=[O:15])=[CH:10][C:9]=1[N+:16]([O-:18])=[O:17])[CH2:4][C:5]([OH:7])=[O:6])[CH3:2].C(O)C.[BH4-].[Na+].C(O)(=O)C>O>[CH2:1]([N:3]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][OH:15])=[CH:10][C:9]=1[N+:16]([O-:18])=[O:17])[CH2:4][C:5]([OH:7])=[O:6])[CH3:2]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 702EthanolHCID 4311764Sodium borohydrideHCID 86743322ethyl N-(4-formyl-2-nitrophenyl)glycine

생성물 1

HCID 70396304HCID 70396304, 화합물수율 70.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

(a-2) To a stirred solution of 47.8 parts of ethyl N-(4-formyl-2-nitrophenyl)glycine in 280 parts of ethanol were added in small portions 3.8 parts of sodium tetrahydroborate. The whole was stirred for 30 minutes at room temperature. The reaction mixture was decomposed by a solution of 12 parts of acetic acid in 50 parts of water. The mixture was concentrated. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was crystallized from 2-propanol. The product was filtered off and dried, yielding 34.1 parts (70.6%) of ethyl N-[4-(hydroxymethyl)-2-nitrophenyl]glycine (int. 30).

후처리

  1. concentrationThe mixture was concentrated
  2. extractionThe product was extracted with dichloromethane
  3. customThe extract was dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was crystallized from 2-propanol
  7. filtrationThe product was filtered off
  8. customdried

출처 및 근거

ORD 기록
ord-395036b3f628442ea1aaf8df603af093
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04859684

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