Formic Acid → HCID 13060164、化合物

HRID 1982678ノート

反応式

HRID 1982678 の反応式
[C:1](OC(=O)C)(=[O:3])C.C(O)=O.[NH2:11][C:12]1[N:17]=[C:16]([CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:15]=[CH:14][CH:13]=1.O>C(OCC)(=O)C>[CH:1]([NH:11][C:12]1[N:17]=[C:16]([CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:15]=[CH:14][CH:13]=1)=[O:3]

参加物

6

反応物 4

HCID 284Formic AcidHCID 962WaterHCID 7918Acetic AnhydrideHCID 13060163Ethyl (6-aminopyridin-2-yl)acetate

生成物 1

HCID 13060164HCID 13060164、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Acetic anhydride (16.6 ml.) and 98% formic acid (7.32 ml.) were mixed at room temperature and stirred at 50° to 66° C. for 30 minutes. The solution was dropwise added to a solution of ethyl 2-(6-aminopyridin-2-yl)acetate (26.5 g.) in ethyl acetate (250 ml.) at 20° to 23° C. over 30 minutes, and stirred at the same temperature for one hour. Cool water was added to the resultant solution and shaked sufficiently. The ethyl acetate layer was separated, washed with water, an aqueous solution of sodium bicarbonate and water in turn, dried and concentrated under reduced pressure to give ethyl 2-(6-formamidopyridin-2-yl)acetate (28 g.), mp 35° to 38° C.

後処理

  1. stirringstirred at the same temperature for one hour
  2. customThe ethyl acetate layer was separated
  3. washwashed with water
  4. dry with materialan aqueous solution of sodium bicarbonate and water in turn, dried
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-7c93147beff6473092bf8dbe7f572141
出典データセット
uspto-grants-1986_06
特許番号
US04596869

反応ノート

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