Water → Pyridine-2-carbothioamide

HRID 1682425

反応式

HRID 1682425 の反応式
P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:2].[NH2:15][C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=1)=O.O>O1CCCC1>[N:19]1[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=1[C:16](=[S:2])[NH2:15]

参加物

5

反応物 3

HCID 962WaterHCID 14817Phosphorus sulfide (P2S5)HCID 150702-Pyridinecarboxamide

生成物 1

HCID 1549499Pyridine-2-carbothioamide収率 74.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

43 g of phosphorus pentasulfide were added slowly to 46.8 g of the amide of Stage A in 700 ml of tetrahydrofuran and the mixture was stirred for 4 hours at ambient temperature. The reaction mixture was poured into water and extracted with ether. The extracts were dried and the solvent was evaporated under reduced pressure. After chromatography on silica (eluant: CH2Cl2 --AcOEt 8-2), 10 g of expected product melting at 137° C. were obtained.

後処理

  1. extractionextracted with ether
  2. customThe extracts were dried
  3. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-189d08015cd14c07b7bc2532edc628c1
出典データセット
uspto-grants-1997_06
特許番号
US05635485

関連ノート

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