Dabco → HCID 21539297, 화합물

HRID 1076227노트

반응식

HRID 1076227 반응식
[CH2:1]1[C:6]2([C:15](=[S:16])[NH:14][C:8]3([CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]3)[NH:7]2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:17][N:18]=[C:19]=[O:20].N12CCN(CC1)CC2>C1C=CC=CC=1>[CH3:17][NH:18][C:19]([N:14]1[C:15](=[S:16])[C:6]2([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5]2)[NH:7][C:8]21[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]2)=[O:20]

참가 물질

5

반응물 3

HCID 9237DabcoHCID 12228Methyl Isocyanate2회HCID 853997NSC515893

생성물 1

HCID 21539297HCID 21539297, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

4.8 Parts of 7,14-diazadispiro[5.1.5.2]pentadecane-15-thione, 2.28 parts of methyl isocyanate and a trace of 1,4-diazabicyclo[2.2.2]octane in 100 parts of dry benzene were heated at reflux for 4 days. A further 2.28 parts of methyl isocyanate were added and the solution again heated at reflux for 16 hours. The solvent was then evaporated in vacuo and the residue was crystallised twice from ethyl acetate to give 14-methylcarbamoyl-7,14-diazadispiro[5.1.5.2]pentadecane-15-thione as a colourless solid of melting point 127° to 129°C. This material gave the following elemental analysis by weight:

후처리

  1. temperatureat reflux for 4 days
  2. temperaturethe solution again heated
  3. temperatureat reflux for 16 hours
  4. customThe solvent was then evaporated in vacuo
  5. customthe residue was crystallised twice from ethyl acetate

출처 및 근거

ORD 기록
ord-ad25879a620b44bdb3012342bd2e4636
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03956310

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