Methyl Isocyanate → 1,3-Dimethyl-3-[5-(beta-chloro-alpha,alpha-dimethylethyl)-1,3,4-thiadiazol-2-yl]urea
反応式
[CH3:1][NH:2][C:3]1[S:4][C:5]([C:8]([CH3:12])([CH3:11])[CH2:9][Cl:10])=[N:6][N:7]=1.[CH3:13][N:14]=[C:15]=[O:16]>C1C=CC=CC=1>[CH3:13][NH:14][C:15]([N:2]([CH3:1])[C:3]1[S:4][C:5]([C:8]([CH3:11])([CH3:12])[CH2:9][Cl:10])=[N:6][N:7]=1)=[O:16]参加物
4
実験手順
To a stirred suspension of 6.0 g of 2-methylamino-5-(β-chloro-α,α-dimethylethyl)-1,3,4-thiadiazole in 100 ml of benzene was added 2.0 g of methyl isocyanate. The mixture became homogenous upon heating to reflux temperature and reflux was maintained for 2 hrs. After cooling, the benzene was removed at reduced pressure and the precipitate collected, giving 7.4 g (95%), m.p. 159°-161°. An analytical sample was prepared from methylene chloride-ether, m.p. 160°-161°.
後処理
- temperatureupon heating
- temperatureto reflux temperature
- temperaturereflux
- temperaturewas maintained for 2 hrs
- temperatureAfter cooling
- customthe benzene was removed at reduced pressure
- customthe precipitate collected
- customgiving 7.4 g (95%), m.p. 159°-161°
出典と根拠
- ORDレコード
- ord-3d86097b63644da486159aa017099551
- 出典データセット
- uspto-grants-1978_06
- 特許番号
- US04097264
反応ノート
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