Acetic Acid → HCID 70396304、化合物

HRID 1723097

反応式

HRID 1723097 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 70396304HCID 70396304、化合物収率 70.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

(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).

後処理

  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

出典と根拠

ORDレコード
ord-395036b3f628442ea1aaf8df603af093
出典データセット
uspto-grants-1989_08
特許番号
US04859684

関連ノート

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