Water → HCID 19974642、化合物

HRID 1451641ノート

反応式

HRID 1451641 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][C:11]1[CH:19]=[CH:18][C:17]([S:20][CH3:21])=[CH:16][C:12]=1[C:13]([OH:15])=[O:14])([OH:3])=O.O>P(Cl)(Cl)(Cl)=O>[CH3:21][S:20][C:17]1[CH:16]=[C:12]([C:13]([OH:15])=[O:14])[C:11]2[NH:10][C:5]3[C:4](=[CH:9][CH:8]=[CH:7][CH:6]=3)[C:1](=[O:3])[C:19]=2[CH:18]=1

参加物

4

反応物 2

HCID 962WaterHCID 19974595HCID 19974595、化合物

生成物 1

HCID 19974642HCID 19974642、化合物

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

The product of part (i) above (2 g) in phosphorus oxychloride (6 ml) was heated at reflux for 1 h. The solution was then cooled (to 0°), and water (15 ml) was added slowly. The mixture was then heated at 100° for 10 min and then poured onto cracked ice. The resulting precipitate was filtered off, washed with water, and crystallised from methanol to give the title compound (1.6 g). IR includes peaks at 1690 cm-1 (CO2H) and 1620 cm-1 (CO).

後処理

  1. temperatureat reflux for 1 h
  2. additionwas added slowly
  3. temperatureThe mixture was then heated at 100° for 10 min
  4. additionpoured
  5. filtrationThe resulting precipitate was filtered off
  6. washwashed with water
  7. customcrystallised from methanol

出典と根拠

ORDレコード
ord-76c77db7d62247a1b4d752a6666c52e5
出典データセット
uspto-grants-1997_02
特許番号
US05604237

反応ノート

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