Sodium Hydroxide → 5-Phenylsulfanyl-[1,3,4]thiadiazole-2-carboxylic acid

HRID 1359648ノート

反応式

HRID 1359648 の反応式
C([O:3][C:4]([C:6]1[S:7][C:8]([S:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[N:9][N:10]=1)=[O:5])C.[OH-].[Na+]>CCO>[C:12]1([S:11][C:8]2[S:7][C:6]([C:4]([OH:5])=[O:3])=[N:10][N:9]=2)[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 699746815-Phenylsulfanyl-[1,3,4]thiadiazole-2-carboxylic acid ethyl ester

生成物 1

HCID 181809825-Phenylsulfanyl-[1,3,4]thiadiazole-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The 5-phenylsulfanyl-[1,3,4]thiadiazole-2-carboxylic acid ethyl ester from Step 64a (1.0 g, 3.76 mmol, 1 eq) is dissolved in EtOH (40 mL), and cooled in an ice bath. To this, 2N NaOH (1.88 mL, 3.76 mmol, 1 eq) is added drop wise. The sodium salt of the acid precipitates out of solution. The reaction mixture is concentrated in vacuo to give a white crystalline product. The reaction mixture is carried through to the next step in its crude form to make the acid chloride. MS (ESI) for C9H6N2S2O2 m/z 237.0 (M−H)−.

後処理

  1. temperaturecooled in an ice bath
  2. customThe sodium salt of the acid precipitates out of solution
  3. concentrationThe reaction mixture is concentrated in vacuo
  4. customto give a white crystalline product

出典と根拠

ORDレコード
ord-69024e93a28541f3b6e2e04eba5ae32a
出典データセット
uspto-grants-2003_07
特許番号
US06599916B2

反応ノート

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