HCID 86607107、化合物 → 2-Amino-4-methyl-thiazole-5-sulfonic acid (2-hydroxy-1-hydroxymethyl-ethyl)-amide

HRID 900884ノート

反応式

HRID 900884 の反応式
[OH:1][CH2:2][CH:3]([NH:6][S:7]([C:10]1[S:14][C:13]([NH:15]C(=O)C)=[N:12][C:11]=1[CH3:19])(=[O:9])=[O:8])[CH2:4][OH:5]>Cl>[OH:1][CH2:2][CH:3]([NH:6][S:7]([C:10]1[S:14][C:13]([NH2:15])=[N:12][C:11]=1[CH3:19])(=[O:9])=[O:8])[CH2:4][OH:5]

参加物

3

反応物 1

HCID 86607107HCID 86607107、化合物

生成物 1

HCID 866071082-Amino-4-methyl-thiazole-5-sulfonic acid (2-hydroxy-1-hydroxymethyl-ethyl)-amide収率 44%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
80 °C

実験手順

A stirred suspension of 2-acetamido-4-methyl-thiazole-5-sulfonic acid (2-hydroxy-1-hydroxymethyl-ethyl)-amide (1.45 g, 4.69 mmol) in 6N hydrochloric acid (22 ml) was heated for 2 h at 80° C., evaporated, and saturated NaHCO3 solution (50 ml) was added. The mixture was extracted with ethyl acetate (3×50 ml), the combined organic layers washed with brine (50 ml), dried (MgSO4) and evaporated. The crude product was further purified by crystallization (dichloromethane/MeOH/hexane) to yield the title compound (0.55 g, 44%) as an off-white solid. MS (ISP) 266.0 [(M−H)−].

後処理

  1. customevaporated
  2. additionsaturated NaHCO3 solution (50 ml) was added
  3. extractionThe mixture was extracted with ethyl acetate (3×50 ml)
  4. washthe combined organic layers washed with brine (50 ml)
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customThe crude product was further purified by crystallization (dichloromethane/MeOH/hexane)

出典と根拠

ORDレコード
ord-cc61dda82a3e47d1896adc2260a68dcb
出典データセット
uspto-grants-2008_04
特許番号
US07361659B2

反応ノート

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