Phosgene → HCID 20143943、化合物

HRID 2118432ノート

反応式

HRID 2118432 の反応式
C(N[C:6]([NH:8][S:9]([CH2:12][C:13]1[C:22]([S:23]([N:26]([CH3:28])[CH3:27])(=[O:25])=[O:24])=[CH:21][CH:20]=[CH:19][C:14]=1[C:15]([O:17][CH3:18])=[O:16])(=[O:11])=[O:10])=[O:7])CCC.N12CCN(CC1)CC2.C(Cl)(Cl)=O>>[CH3:27][N:26]([S:23]([C:22]1[CH:21]=[CH:20][CH:19]=[C:14]([C:15]([O:17][CH3:18])=[O:16])[C:13]=1[CH2:12][S:9]([N:8]=[C:6]=[O:7])(=[O:11])=[O:10])(=[O:25])=[O:24])[CH3:28]

参加物

4

反応物 3

HCID 6371PhosgeneHCID 9237DabcoHCID 139376452-[[[(n-Butyl)aminocarbonyl]aminosulfonyl]methyl]-3-(N,N-dimethylamino)sulfonylbenzoic acid, methyl ester

生成物 1

HCID 20143943HCID 20143943、化合物

実験手順

A suspension of 7.4 g of the product from Example 15 and 0.1 g of 1,4-diazabicyclo[2.2.2]octane in 100 ml xylenes was heated to reflux temperature. To this solution was added 1.5 ml of phosgene at a rate that maintained the temperature above 130°. When the addition was complete, the turbid solution was heated at reflux temperature for about one hour, allowed to cool, and then filtered under an atmosphere of nitrogen. Removal of the solvent from the filtrate gave the product as a dark oil which was dissolved in dry methylene chloride and carried on to the next step without purification. The infrared spectrum of this intermediate displayed a characteristic isocyanate absorption at 2240 cm-1.

後処理

  1. temperaturewas heated
  2. temperatureto reflux temperature
  3. temperaturemaintained the temperature above 130°
  4. additionWhen the addition
  5. temperaturethe turbid solution was heated
  6. temperatureat reflux temperature for about one hour
  7. temperatureto cool
  8. filtrationfiltered under an atmosphere of nitrogen
  9. customRemoval of the solvent from the filtrate

出典と根拠

ORDレコード
ord-a526caeb438b441296c8ee4669a0c2fc
出典データセット
uspto-grants-1987_07
特許番号
US04678500

反応ノート

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