Methanol → Methyl 3-isocyanatopropanoate

HRID 720214ノート

反応式

HRID 720214 の反応式
S(O)(O)(=O)=O.[CH3:6][O:7][C:8](=[O:12])[CH2:9][CH2:10][NH2:11].CO.C(N(CC)CC)C.[CH2:22]([O:24]C(Cl)=O)C>C(OCC)(=O)C.C(=S)=S>[CH3:6][O:7][C:8]([CH2:9][CH2:10][N:11]=[C:22]=[O:24])=[O:12]

参加物

7

反応物 4

HCID 887MethanolHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 21889522HCID 21889522、化合物

生成物 1

HCID 2769480Methyl 3-isocyanatopropanoate収率 89.3%

試薬・触媒・溶媒 2

HCID 6348Carbon Disulfide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution containing 603.6 g of β-alanine-methylester sulfate and 1.5 liter of methyl alcohol, 1,256 ml of triethylamine was added at a freezing point and thereto, 235 ml of carbon disulfide was added dropwise at 10° C. or less. After the dropwise addition, the solution was stirred at 10° C. or less for 1 hour and then 288 ml of ethylchloroformate was added dropwise and in this state, the solution was stirred for 2 hours. After the reaction, the reaction solution was subjected to liquid separation with ethyl acetate and water. The extracted ethyl acetate layer was dried over magnesium sulfate and filtered and then the ethyl acetate was removed by distillation under reduced pressure to 389.1 g (yield: 89.3%) of the objective compound as an oily product.

後処理

  1. additionwas added at a freezing point
  2. additionAfter the dropwise addition
  3. stirringthe solution was stirred for 2 hours
  4. customAfter the reaction
  5. customthe reaction solution was subjected to liquid separation with ethyl acetate and water
  6. dry with materialThe extracted ethyl acetate layer was dried over magnesium sulfate
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-6ecbaed300d749deb642809dba1c87a4
出典データセット
uspto-grants-2006_11
特許番号
US07135275B2

反応ノート

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