Phosgene → 2-Nitrophenylmethanesulfonyl isocyanate

HRID 904771ノート

反応式

HRID 904771 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH2:10][S:11]([NH2:14])(=[O:13])=[O:12])([O-:3])=[O:2].C(N=[C:20]=[O:21])CCC.C1N2CCN(CC2)C1.C(Cl)(Cl)=O>>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH2:10][S:11]([N:14]=[C:20]=[O:21])(=[O:12])=[O:13])([O-:3])=[O:2]

参加物

5

反応物 4

HCID 6371PhosgeneHCID 8110Butyl isocyanateHCID 9237DabcoHCID 13266249(2-Nitrophenyl)methanesulfonamide

生成物 1

HCID 132826592-Nitrophenylmethanesulfonyl isocyanate

実験手順

A solution of 9.0 g of the product of Example 3, 4.2 g of butyl isocyanate and 0.1 g of DABCO in 80 ml of dry xylenes was heated to 136°. To this solution was added 3.0 ml of liquid phosgene at such a rate as to maintain the temperature between 125° and 136°. This addition required about 21/2 hours. The solution was cooled to 25°, filtered under nitrogen and stripped in vacuo to give crude 2-nitrophenylmethanesulfonyl isocyanate as a viscous, moisture-sensitive oil showing a sulfonyl isocyanate peak in the infrared at 2230 cm-1.

後処理

  1. temperatureto maintain the temperature between 125° and 136°
  2. additionThis addition
  3. custom2 hours
  4. temperatureThe solution was cooled to 25°
  5. filtrationfiltered under nitrogen

出典と根拠

ORDレコード
ord-9ab3802cc35440d0978923ddc42a190c
出典データセット
uspto-grants-1983_12
特許番号
US04420325

反応ノート

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