Lithium Hydroxide → 4-((6-(2-(dimethylamino)-1-(1H-imidazol-1-yl)butyl)benzo[d]thiazol-2-yl)carbamoyl)benzoic acid

HRID 538878ノート

反応式

HRID 538878 の反応式
[CH3:1][N:2]([CH3:34])[CH:3]([CH2:32][CH3:33])[CH:4]([C:10]1[CH:31]=[CH:30][C:13]2[N:14]=[C:15]([NH:17][C:18]([C:20]3[CH:29]=[CH:28][C:23]([C:24]([O:26]C)=[O:25])=[CH:22][CH:21]=3)=[O:19])[S:16][C:12]=2[CH:11]=1)[N:5]1[CH:9]=[CH:8][N:7]=[CH:6]1.[OH-].[Li+]>O1CCOCC1.O>[CH3:1][N:2]([CH3:34])[CH:3]([CH2:32][CH3:33])[CH:4]([C:10]1[CH:31]=[CH:30][C:13]2[N:14]=[C:15]([NH:17][C:18]([C:20]3[CH:29]=[CH:28][C:23]([C:24]([OH:26])=[O:25])=[CH:22][CH:21]=3)=[O:19])[S:16][C:12]=2[CH:11]=1)[N:5]1[CH:9]=[CH:8][N:7]=[CH:6]1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 54760442methyl 4-((6-(2-(dimethylamino)-1-(1H-imidazol-1-yl)butyl)benzo[d]thiazol-2-yl)carbamoyl)benzoate

生成物 1

HCID 547602554-((6-(2-(dimethylamino)-1-(1H-imidazol-1-yl)butyl)benzo[d]thiazol-2-yl)carbamoyl)benzoic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
50 °C

実験手順

A mixture of methyl 4-((6-(2-(dimethylamino)-1-(1H-imidazol-1-yl)butyl)benzo[d]thiazol-2-yl)carbamoyl)benzoate (15 mg, 0.031 mmol) and lithium hydroxide (6.6 mg, 0.157 mmol) in dioxane (2 mL) and water (1 mL) was stirred at 50° C. for 4 h. The reaction was evaporated, water was added and neutralized to pH 7. The slurry obtained was evaporated and extracted with DCM-methanol mixture and evaporated. The crude acid was purified by PTLC using DCM-methanol mixture as eluent to afford 4-((6-(2-(dimethylamino)-1-(1H-imidazol-1-yl)butyl)benzo[d]thiazol-2-yl)carbamoyl)benzoic acid. MS ESI: m/462.11 [M−1−].

後処理

  1. customThe reaction was evaporated
  2. additionwater was added
  3. customThe slurry obtained
  4. customwas evaporated
  5. extractionextracted with DCM-methanol mixture
  6. customevaporated
  7. customThe crude acid was purified by PTLC

出典と根拠

ORDレコード
ord-226ba5a41943413097a543009669f4af
出典データセット
uspto-grants-2014_10
特許番号
US08865752B2

反応ノート

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