Sodium Hydroxide → 1H-Thieno[2,3-d]imidazole-5-carboxylic acid, 2-(methoxymethyl)-1-methyl-

HRID 50381

反応式

HRID 50381 の反応式
[CH3:1][N:2]1[C:6]2[CH:7]=[C:8]([C:10]([O:12]CC)=[O:11])[S:9][C:5]=2[N:4]=[C:3]1[CH2:15][O:16][CH3:17].[OH-].[Na+]>C(O)C>[CH3:1][N:2]1[C:6]2[CH:7]=[C:8]([C:10]([OH:12])=[O:11])[S:9][C:5]=2[N:4]=[C:3]1[CH2:15][O:16][CH3:17]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 18412470Ethyl 1-methyl-2-methoxymethylthieno[2,3-d]imidazol-5-yl-carboxylate

生成物 1

HCID 184123181H-Thieno[2,3-d]imidazole-5-carboxylic acid, 2-(methoxymethyl)-1-methyl-

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 0.90 g (3.54 mmol) of ethyl 1-methyl-2-methoxymethylthieno[2,3-d]imidazol-5-yl-carboxylate in 30 mL of ethanol were added dropwise 5 mL of 2 N sodium hydroxide solution and the mixture was stirred for 2 hours at ambient temperature. Then the solvent was distilled off in vacuo, the residue was taken up in 5 mL of water and washed with 10 mL of diethylether. The aqueous phase was acidified with 6 mL of 2N hydrochloric acid, cooled to 0° C. and the precipitated crystals are filtered off. Yield: 0.50 g (63% of theory), C9H10N2O3S (226.26); Rf value: 0.21 (silica gel; methylene chloride/ethanol=9:1+a few drops of acetic acid); mass spectrum: (M)+=226.

後処理

  1. distillationThen the solvent was distilled off in vacuo
  2. washwashed with 10 mL of diethylether
  3. temperaturecooled to 0° C.
  4. filtrationthe precipitated crystals are filtered off

出典と根拠

ORDレコード
ord-ead789528f834d4bbb98b032d632c338
出典データセット
uspto-grants-2004_03
特許番号
US06710055B2

関連ノート

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