Methyl Isocyanate → Monoisouron

HRID 1155478ノート

反応式

HRID 1155478 の反応式
[CH3:1][C:2]([C:5]1[O:9][N:8]=[C:7]([NH2:10])[CH:6]=1)([CH3:4])[CH3:3].[CH3:11][N:12]=[C:13]=[O:14]>CN(C)C1C=CN=CC=1.C1C=CC=CC=1>[CH3:1][C:2]([C:5]1[O:9][N:8]=[C:7]([NH:10][C:13]([NH:12][CH3:11])=[O:14])[CH:6]=1)([CH3:4])[CH3:3]

参加物

5

反応物 2

HCID 12228Methyl IsocyanateHCID 1714733-Isoxazolamine, 5-(1,1-dimethylethyl)-

生成物 1

HCID 186687Monoisouron収率 72.4%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 241Benzene溶媒2 回

実験手順

A 50 milliliter flask with a magnetic stirring bar, addition funnel, thermometer and condenser/drying tube was charged with 3.0 grams (0.021 mole) of 5-(1,1-dimethylethyl)-3-isoxazolamine, a few crystals of 4-dimethylaminopyridine and 20 milliliters of benzene. The funnel was charged with 2.3 grams (0.040 mole) of methyl isocyanate in 5 milliliters of benzene, which was added dropwise over five (5) minutes. After standing overnight, the mass of crystals which formed was isolated by filtration, washed with hexane, and air dried to give 3.0 grams of white powder of 1-[5-(1,1-dimethylethyl)-3-isoxazolyl]-3-methylurea, M.P. 188°-189° C.

後処理

  1. additionA 50 milliliter flask with a magnetic stirring bar, addition funnel
  2. customthermometer and condenser/drying tube
  3. customthe mass of crystals which formed
  4. customwas isolated by filtration
  5. washwashed with hexane, and air
  6. customdried

出典と根拠

ORDレコード
ord-ab3df0f911a54ac28b1b4b932fc9a9bf
出典データセット
uspto-grants-1981_11
特許番号
US04302239

反応ノート

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