Diethyl Ether → HCID 136088519、化合物

HRID 227656ノート

反応式

HRID 227656 の反応式
[NH2:1][C:2]1[S:3][C:4]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:5]([OH:7])[N:6]=1.[C:13](OC(=O)C)(=[O:15])[CH3:14].C(OCC)C>C(O)(=O)C>[C:13]([NH:1][C:2]1[S:3][C:4]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:5]([OH:7])[N:6]=1)(=[O:15])[CH3:14]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 7918Acetic AnhydrideHCID 224465Ethyl 2-amino-4-hydroxythiazole-5-carboxylate

生成物 1

HCID 136088519HCID 136088519、化合物収率 82.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Ethyl 2-amino-4-hydroxy-1,3-thiazole-5-carboxylate (6.00 g, 31.9 mmol) was dissolved in 100 mL of acetic acid with stirring. Acetic anhydride (15.0 mL, 159 mmol) was added via syringe. The reaction was stirred for 16 hours and 100 mL of diethyl ether was added. The reaction was filtered and the pale yellow solid was washed with diethyl ether, dried, and collected to afford 6.04 g (82%) of ethyl 2-(acetylamino)-4-hydroxy-1,3-thiazole-5-carboxylate. 1H NMR (300 MHz, DMSO-d6) δ 12.32 (s, 1H), 11.32 (s, 1H), 4.16 (q, J=7.0 Hz, 2H), 2.16 (s, 3H), 1.23 (t, J=7.0 Hz, 3H).

後処理

  1. stirringThe reaction was stirred for 16 hours
  2. filtrationThe reaction was filtered
  3. washthe pale yellow solid was washed with diethyl ether
  4. customdried
  5. customcollected

出典と根拠

ORDレコード
ord-5bb04ea29b194249901b37581aa15972
出典データセット
uspto-grants-2009_07
特許番号
US07560568B2

反応ノート

読み込み中…