Water → (2Z)-2-(2-amino-1,3-thiazol-4-yl)-2-[2-(diethylamino)-2-oxoethoxy]iminoacetic acid

HRID 1195069ノート

反応式

HRID 1195069 の反応式
[NH2:1][C:2]1[S:3][CH:4]=[C:5](/[C:7](=[N:13]/[O:14][CH2:15][C:16](=[O:22])[N:17]([CH2:20][CH3:21])[CH2:18][CH3:19])/[C:8]([O:10]CC)=[O:9])[N:6]=1.O.[OH-].[Na+]>CO>[NH2:1][C:2]1[S:3][CH:4]=[C:5](/[C:7](=[N:13]/[O:14][CH2:15][C:16](=[O:22])[N:17]([CH2:20][CH3:21])[CH2:18][CH3:19])/[C:8]([OH:10])=[O:9])[N:6]=1

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 21269044HCID 21269044、化合物

生成物 1

HCID 21269034(2Z)-2-(2-amino-1,3-thiazol-4-yl)-2-[2-(diethylamino)-2-oxoethoxy]iminoacetic acid収率 402.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

68.1 g of ethyl 2-(2-amino-4-thiazolyl)-2-[(Z)-[(diethylcarbamoyl)methoxy]imino]-acetate are dissolved in 2.8 l of methanol and 240 ml of water and the solution is treated with 230 ml of 1N aqueous sodium hydroxide solution. The methanol is removed under reduced pressure after 48 hours and the aqueous solution is washed with ethyl acetate. After the addition of 230 ml of 1N aqueous hydrochloric acid, the crystallized acid is filtered off and dried. There are obtained 250.8 g of 2-(2-amino-4-thiazolyl)-2-[(Z)-[(diethylcarbamoyl)methoxy]imino]-acetic acid of melting point 180° C.

後処理

  1. customThe methanol is removed under reduced pressure after 48 hours
  2. washthe aqueous solution is washed with ethyl acetate
  3. additionAfter the addition of 230 ml of 1N aqueous hydrochloric acid
  4. filtrationthe crystallized acid is filtered off
  5. customdried

出典と根拠

ORDレコード
ord-5730ed26a10b48a099a3cbc4a33b42f2
出典データセット
uspto-grants-1989_03
特許番号
US04816582

反応ノート

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