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Phosgene → 1-(3-Isocyanatophenyl)-3,3-dimethylpyrrolidine-2,5-dione

HRID 435045
ノート
印刷プレビュー

反応式

HRID 435045 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12](=[O:13])[CH2:11][C:10]([CH3:15])([CH3:14])[C:9]2=[O:16])[CH:5]=[CH:6][CH:7]=1.C(N(CC)CC)C.[C:24](Cl)(Cl)=[O:25]>O1CCCC1>[N:1]([C:2]1[CH:3]=[C:4]([N:8]2[C:12](=[O:13])[CH2:11][C:10]([CH3:14])([CH3:15])[C:9]2=[O:16])[CH:5]=[CH:6][CH:7]=1)=[C:24]=[O:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6371PhosgeneHCID 8471TriethylamineHCID 13189216N-m-AMINOPHENYL-2,2-DIMETHYLSUCCINIMIDE

生成物 1

HCID 131892331-(3-Isocyanatophenyl)-3,3-dimethylpyrrolidine-2,5-dione

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Seventy-three g. of N-m-aminophenyl-2,2-dimethylsuccinimide, as prepared in Example II, was dissolved in 800 ml. of tetrahydrofuran containing 75 g. of triethylamine, cooled in an ice bath, and added to 60 g. of phosgene in 400 ml. of tetrahydrofuran maintained at about 0° C. in a drying and isopropanol bath. The mixture was allowed to warm to room temperature and the triethylamine hydrochloride was filtered off and the tetrahydrofuran removed under vacuum on the rotary evaporator. Yield was 84 g. of material product having a nD30 of 1.5470. The product was identified as the title compound by analysis of infrared spectra and was used without further purification.

後処理

  1. dissolutionwas dissolved in 800 ml
  2. additionadded to 60 g
  3. filtrationthe triethylamine hydrochloride was filtered off
  4. customthe tetrahydrofuran removed under vacuum on the rotary evaporator
  5. customwas used without further purification

出典と根拠

ORDレコード
ord-acb00831fb814ab2865cb0448d305d2c
出典データセット
uspto-grants-1983_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04400202

反応ノート

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