Water → HCID 21412476, 화합물

HRID 2071798노트

반응식

HRID 2071798 반응식
[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]

참가 물질

6

반응물 4

HCID 962WaterHCID 6367Acetyl chlorideHCID 516892Sodium BicarbonateHCID 21412481HCID 21412481, 화합물

생성물 1

HCID 21412476HCID 21412476, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-10bbc5fa083c4af69dbe8da209c8ec15
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04048326

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