Water → HCID 21412476、化合物

HRID 2071798ノート

反応式

HRID 2071798 の反応式
[C:1](Cl)(=[O:3])[CH3:2].[CH3:5][O:6][C:7]([NH:9][C:10](=[S:27])[NH:11][C:12]1[CH:13]=[C:14]([CH:16]=[CH:17][C:18]=1[NH:19][C:20]([NH:22][C:23]([O:25][CH3:26])=[O:24])=[S:21])[NH2:15])=[O:8].C(=O)(O)[O-].[Na+].O>CC(C)=O>[C:1]([NH:15][C:14]1[CH:16]=[CH:17][C:18]([NH:19][C:20]([NH:22][C:23]([O:25][CH3:26])=[O:24])=[S:21])=[C:12]([NH:11][C:10]([NH:9][C:7]([O:6][CH3:5])=[O:8])=[S:27])[CH:13]=1)(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 962WaterHCID 6367Acetyl chlorideHCID 516892Sodium BicarbonateHCID 21412481HCID 21412481、化合物

生成物 1

HCID 21412476HCID 21412476、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Acetyl chloride (1.66 g; 0.0212 mole) was added dropwise during five minutes to a stirred suspension of 3,4-bis-(3-methoxycarbonyl-2-thioureido)aniline (4.0 g; 0.0112 mole) and sodium bicarbonate (1.78 g; 0.0212 mole) in dry acetone (50 ml). The temperature of the reaction mixture rose spontaneously to 30° C. After completion of the addition, the mixture was refluxed with stirring for 6 hours, cooled and poured into water. The solid which separated was filtered off, washed well with water and crystallised from ethanol to give 4-acetamido-1,2-bis-(3-methoxycarbonyl-2-thioureido)benzene, m.p. 183°-185° C. (with decomposition).

後処理

  1. customrose spontaneously to 30° C
  2. additionAfter completion of the addition
  3. temperaturethe mixture was refluxed
  4. temperaturecooled
  5. customThe solid which separated
  6. filtrationwas filtered off
  7. washwashed well with water
  8. customcrystallised from ethanol

出典と根拠

ORDレコード
ord-10bbc5fa083c4af69dbe8da209c8ec15
出典データセット
uspto-grants-1977_09
特許番号
US04048326

反応ノート

読み込み中…