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Cis-4-thiocyano-3-buten-2-one → HCID 178467920, 화합물

HRID 1463791
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HRID 1463791 반응식
O.[Na].[SH:3][C:4]1[N:8]([CH3:9])[N:7]=[N:6][N:5]=1.S(/[CH:13]=[CH:14]\[C:15](=[O:17])[CH3:16])C#N>C(O)C>[SH:3][C:4]1[N:8]([CH3:9])[N:7](/[CH:13]=[CH:14]\[C:15](=[O:17])[CH3:16])[NH:6][N:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 45085240Cis-4-thiocyano-3-buten-2-one2회HCID 178482031HCID 178482031, 화합물

생성물 1

HCID 178467920HCID 178467920, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

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온도
25 °C

실험 절차

To a stirred solution of 5-mercapto-1-methyltetrazole sodium salt hydrate (1.1 g., 0.008 mole) in aqueous ethanol (15 ml), a solution of cis-4-thiocyano-3-buten-2-one (Compound 28) in ethanol was added dropwise over 5 minutes. A solid suspension was observed forming over the next 2 hours which was stirred at 25° C. for 18 hours. The volatiles were removed in vacuo and the residue was extracted into ethyl acetate and washed thoroughly with water. After drying (MgSO4), the solution was concentrated. The solid residue was purified via column chromatography on silica gel using hexanes/ethyl acetate (3:2) as eluant to yield 1.1 g of a white solid, mp 112°-114° C. IR (nujol) uc=o 1660 cm-1.

후처리

  1. customA solid suspension was observed forming over the next 2 hours which
  2. customThe volatiles were removed in vacuo
  3. extractionthe residue was extracted into ethyl acetate
  4. washwashed thoroughly with water
  5. dry with materialAfter drying (MgSO4)
  6. concentrationthe solution was concentrated
  7. customThe solid residue was purified via column chromatography on silica gel

출처 및 근거

ORD 기록
ord-ed9be222d7c344df9a075c8e40d5a5bb
출처 데이터셋
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05302592

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