Dichloromethane → HCID 178448704、化合物

HRID 1199746ノート

反応式

HRID 1199746 の反応式
[CH2:1]([N:5]1[C:12](=[O:13])[CH2:11][C:9](=[O:10])[N:8]([CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[C:6]1=[O:7])[CH2:2][CH2:3][CH3:4].C1(C)C=CC(S([N:29]=[N+:30]=[N-])(=O)=O)=CC=1.C(N(CC)CC)C.ClCCl>C(#N)C>[CH2:1]([N:5]1[C:12](=[O:13])[C:11](=[N+:29]=[N-:30])[C:9](=[O:10])[N:8]([CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[C:6]1=[O:7])[CH2:2][CH2:3][CH3:4]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 13661p-Toluenesulfonyl azideHCID 14848100HCID 14848100、化合物

生成物 1

HCID 178448704HCID 178448704、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

反応条件

温度
2 °C

実験手順

80 mL of reagent grade acetonitrile and 6.65 gm (0.025 mole) of 1-(1-butyl)-3-cyclohexylbarbituric acid were added to a dry 250 mL 3-neck round bottom flask equipped with a thermometer, pressure equalizing dropping funnel capped by a drying tube, nitrogen inlet and magnetic stirrer. The stirred solution was cooled to 2° C. in an ice bath. Then a solution of 5.75 gm (0.029 mole) of p-toluenesulfonyl azide in 20 mL of acetonitrile was added to the reaction flask. A solution of 3.20 gm (0.0317 mole) of triethylamine in 20 mL of reagent grade dichloromethane was placed in the dropping funnel and slowly added to the reaction flask, while keeping the temperature below 3° C. The flask temperature was kept below 3° C. for 1 hour. The stirred reaction flask was allowed to warm to room temperature (20° C.) and kept at room temperature for 12 hours.

後処理

  1. customequipped with a thermometer, pressure
  2. customcapped by a drying tube, nitrogen inlet and magnetic stirrer
  3. additionslowly added to the reaction flask
  4. customthe temperature below 3° C
  5. customThe stirred reaction flask
  6. temperatureto warm to room temperature (20° C.)
  7. waitkept at room temperature for 12 hours

出典と根拠

ORDレコード
ord-a3aaf410ba904e71b671db5787ec800e
出典データセット
uspto-grants-1990_02
特許番号
US04902784

反応ノート

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