Phosgene → 3-Acetyl-1-Chlorocarbonyl-2-Imidazolidone

HRID 1282740ノート

反応式

HRID 1282740 の反応式
[C:1]([N:4]1[CH2:8][CH2:7][NH:6][C:5]1=[O:9])(=[O:3])[CH3:2].C(N(CC)CC)C.C[Si](C)(C)Cl.[C:22](Cl)([Cl:24])=[O:23]>C1C=CC=CC=1>[C:1]([N:4]1[CH2:8][CH2:7][N:6]([C:22]([Cl:24])=[O:23])[C:5]1=[O:9])(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 6371PhosgeneHCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 79350N-Acetylimidazolidinone

生成物 1

HCID 112292653-Acetyl-1-Chlorocarbonyl-2-Imidazolidone

試薬・触媒・溶媒 1

HCID 241Benzene溶媒3 回

実験手順

20 parts by weight of N-acetyl-imidazolid-2-one mixed with 25 parts by weight of triethylamine and 150 parts by volume of dry benzene were first taken and 27 parts by weight of trimethylchlorosilane in 40 parts by volume of benzene were added dropwise at room temperature over the course of 30 minutes, with stirring. The mixture was subsequently boiled for 18 hours under reflux, moisture being excluded, and the triethylamine hydrochloride which precipitated (22 parts by weight = 100%) was filtered off after cooling and carefully rinsed with dry benzene. The benzene solution thus obtained was treated with a solution of 17 parts by weight of phosgene in 50 parts by volume of benzene at 5° C and left to stand overnight at 5° C. Thereafter the solvent was stripped off in vacuo and the residue was dried under an oil pump. It was recrystallized from acetone/pentane mixture.

後処理

  1. temperatureunder reflux
  2. customthe triethylamine hydrochloride which precipitated (22 parts by weight = 100%)
  3. filtrationwas filtered off
  4. temperatureafter cooling
  5. washcarefully rinsed with dry benzene
  6. customThe benzene solution thus obtained
  7. waitleft
  8. waitto stand overnight at 5° C
  9. customthe residue was dried under an oil pump
  10. customIt was recrystallized from acetone/pentane mixture

出典と根拠

ORDレコード
ord-3f501c2ce58d4a2c81760f79440b391b
出典データセット
uspto-grants-1976_08
特許番号
US03972870

反応ノート

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