Ethanol → HCID 178527970、化合物

HRID 732030ノート

反応式

HRID 732030 の反応式
[CH:1]([NH:3][NH2:4])=O.[N:5]([CH2:8][C:9]1[O:10][CH:11]=[CH:12][CH:13]=1)=[C:6]=[S:7].C(O)C>N1C=CC=CC=1>[O:10]1[CH:11]=[CH:12][CH:13]=[C:9]1[CH2:8][N:5]1[CH:1]=[N:3][N:4]=[C:6]1[SH:7]

参加物

5

反応物 3

HCID 702EthanolHCID 12229HydrazinecarboxaldehydeHCID 783802-(Isothiocyanatomethyl)furan

生成物 1

HCID 178527970HCID 178527970、化合物収率 83.7%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

実験手順

A solution of formic acid hydrazide (439 mg, 7.809 mmol) in pyridine (20 ml) was added to a solution of 2-isothiocyanatomethyl-furan (1 g, 7.185 mmol) in pyridine (20 ml). Reaction took place at room temperature overnight, and ethanol (20 ml) was added directly to the reaction and placed in 80C bath overnight. Solvent was evaporated and the title compound (1.09 g, 83%) was obtained from purification by SPE chromatography on silica gel with 500 ml 20%, 250 ml 25%, 250 ml 30%, 250 ml 35%, 250 ml 40%, and 250 ml 50% ethyl acetate in hexanes. 1H NMR (CD3OD), δ (ppm): 14.0 (bs, 1H), 8.19 (s, 1H), 7.52 (q, 1H), 6.52 (m, 1H), 6.42 (m, 1H), 4.90 (s, 2H).

後処理

  1. customReaction
  2. customat room temperature
  3. additionwas added directly to the reaction
  4. customSolvent was evaporated

出典と根拠

ORDレコード
ord-fddb11e2fa3d415cbcf778f8e2af7f3b
出典データセット
uspto-grants-2009_09
特許番号
US07585881B2

反応ノート

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