Formic Acid → N-[1-[3-(Formyloxy)propyl]-1H-pyrazol-5-yl]formamide

HRID 2082025ノート

反応式

HRID 2082025 の反応式
[NH2:1][C:2]1[N:6]([CH2:7][CH2:8][CH2:9][OH:10])[N:5]=[CH:4][CH:3]=1.[C:11](OC(=O)C)(=[O:13])C.[CH:18](O)=[O:19].C(=O)([O-])[O-].[K+].[K+]>O1CCCC1.C(OCC)(=O)C>[CH:11]([NH:1][C:2]1[N:6]([CH2:7][CH2:8][CH2:9][O:10][CH:18]=[O:19])[N:5]=[CH:4][CH:3]=1)=[O:13]

参加物

7

反応物 4

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 14996572HCID 14996572、化合物

生成物 1

HCID 14996573N-[1-[3-(Formyloxy)propyl]-1H-pyrazol-5-yl]formamide

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

5-Amino-1-(3-hydroxypropyl)pyrazole (5.3 g) was added to a mixture of acetic anhydride (8.86 ml) and formic acid (7.08 ml) under ice-cooling. The mixture was stirred for two hours at room temperature. The reaction mixture was added to a mixture of ice-water (30 ml), ethyl acetate (30 ml) and tetrahydrofuran (60 ml), and an aqueous solution of potassium carbonate was added thereto to adjust the pH of the mixture to 7. The organic layer was separated and dried over magnesium sulfate. The magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure to give 5-formamido-1-(3-formyloxypropyl)pyrazole (6.74 g).

後処理

  1. temperaturecooling
  2. customThe organic layer was separated
  3. dry with materialdried over magnesium sulfate
  4. filtrationThe magnesium sulfate was filtered off
  5. customthe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-863e0b7b6bd24580b813e6323876fd3b
出典データセット
uspto-grants-1993_02
特許番号
US05187160

反応ノート

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