Ethanol → HCID 178527970, 화합물

HRID 732030노트

반응식

HRID 732030 반응식
[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]

참가 물질

5

반응물 3

HCID 702EthanolHCID 12229HydrazinecarboxaldehydeHCID 783802-(Isothiocyanatomethyl)furan

생성물 1

HCID 178527970HCID 178527970, 화합물수율 83.7%

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-fddb11e2fa3d415cbcf778f8e2af7f3b
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585881B2

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