Hydrochloric Acid → HCID 54757215, 화합물

HRID 1782157노트

반응식

HRID 1782157 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 54757215HCID 54757215, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6212Chloroform용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6b91ab75ac094a7e9ecc0cda3af0ec4a
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07498333B2

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