Hydrochloric Acid → HCID 54757215、化合物

HRID 1782157ノート

反応式

HRID 1782157 の反応式
[NH2:1][C:2]1[C:3]([CH3:10])=[N:4][S:5][C:6]=1[C:7]([OH:9])=[O:8].[C:11](Cl)(=O)[CH2:12][CH2:13][CH3:14].Cl>N1C=CC=CC=1.C(Cl)(Cl)Cl>[CH3:10][C:3]1[C:2]2[N:1]=[C:11]([CH2:12][CH2:13][CH3:14])[O:8][C:7](=[O:9])[C:6]=2[S:5][N:4]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 8855Butyryl chlorideHCID 228318524-Amino-3-methylisothiazole-5-carboxylic acid

生成物 1

HCID 54757215HCID 54757215、化合物

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6212Chloroform溶媒2 回

実験手順

To a solution of 4-amino-3-methyl-isothiazole-5-carboxylic acid (method 57) (2.91 g, 15 mmol) in pyridine (20 mL) at 0° C., was added dropwise a solution of butyryl chloride (3.18 g, 30 mmol) in chloroform (30 mL). The reaction mixture was allowed to warm to room temperature and stirred overnight. Chloroform (200 mL) was added to the reaction mixture followed by 2M HCl (200 mL) and the mixture was stirred. The chloroform layer was further washed with 2M HCl (100 mL), water (100 mL), brine (100 mL) and concentrated. Column purification of the thus obtained crude product provided the pure product as light brown solid. Yield 2 g (64%). 1H NMR (300 MHz) δ 1.03 (t, 3H), 1.80-1.92 (m, 2H), 2.65 (s, 3H), 2.76 (t, 2H).

後処理

  1. stirringthe mixture was stirred
  2. washThe chloroform layer was further washed with 2M HCl (100 mL), water (100 mL), brine (100 mL)
  3. concentrationconcentrated
  4. customColumn purification of the
  5. customthus obtained crude product

出典と根拠

ORDレコード
ord-6b91ab75ac094a7e9ecc0cda3af0ec4a
出典データセット
uspto-grants-2009_03
特許番号
US07498333B2

反応ノート

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