1,4-Dioxane → 4-Amino-3-methylisothiazole-5-carboxylic acid

HRID 1782156ノート

反応式

HRID 1782156 の反応式
C(OC([NH:8][C:9]1[C:10]([CH3:17])=[N:11][S:12][C:13]=1[C:14]([OH:16])=[O:15])=O)(C)(C)C.O1CCOCC1>Cl>[NH2:8][C:9]1[C:10]([CH3:17])=[N:11][S:12][C:13]=1[C:14]([OH:16])=[O:15]

参加物

4

反応物 2

HCID 312751,4-DioxaneHCID 547572144-((tert-Butoxycarbonyl)amino)-3-methylisothiazole-5-carboxylic acid

生成物 1

HCID 228318524-Amino-3-methylisothiazole-5-carboxylic acid

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

4-tert-Butoxycarbonylamino-3-methyl-isothiazole-5-carboxylic acid (method 56) (11 g, 45 mmol) was dissolved in 50 mL of 4M solution of HCl in 1,4-dioxane (200 mmol) and the resulting solution was stirred at room temperature overnight. The TLC showed the complete disappearance of the starting acid. The reaction was concentrated and the residue was triturated with ether and the precipitated hydrochloride salt was filtered off and washed with ether and dried to provide the product as a light brown powder. Yield 8.2 g (100%). 1H NMR (300 MHz, DMSO-d6) δ 2.30 (s, 3H), 8.85 (bs, 3H).

後処理

  1. concentrationThe reaction was concentrated
  2. customthe residue was triturated with ether
  3. filtrationthe precipitated hydrochloride salt was filtered off
  4. washwashed with ether
  5. customdried

出典と根拠

ORDレコード
ord-e7dc112e99194e489a6f48d4466c973a
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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