Potassium Carbonate → 9H-Thioxanthen-9-one, 1-[[2-(dimethylamino)ethyl]amino]-4-nitro-

HRID 1380614노트

반응식

HRID 1380614 반응식
[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][NH2:5].Cl[C:8]1[C:21]2[C:20](=[O:22])[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[S:13][C:12]=2[C:11]([N+:23]([O-:25])=[O:24])=[CH:10][CH:9]=1.C([O-])([O-])=O.[K+].[K+]>C1(C)C(C)=CC=CC=1>[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][NH:5][C:8]1[C:21]2[C:20](=[O:22])[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[S:13][C:12]=2[C:11]([N+:23]([O-:25])=[O:24])=[CH:10][CH:9]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 66053N,N-Dimethylethylenediamine2회HCID 12909396HCID 12909396, 화합물

생성물 1

HCID 3296019H-Thioxanthen-9-one, 1-[[2-(dimethylamino)ethyl]amino]-4-nitro-수율 85.6%

시약·촉매·용매 1

HCID 7237O-Xylene용매2회

실험 절차

A solution of 9.3 g (0.105 mole) of N,N-dimethylethylenediamine in 35 ml of xylene was added dropwise over ten minutes to a stirred mixture of 1-chloro-4-nitrothioxanthone (24.5 g, 0.084 mole) and K2CO3 (12.2 g, 0.088 mole) in 350 ml of xylene. The mixture was heated for one hour at 70°, an additional 1.8 g (0.088 mole) of N,N-dimethylethylendiamine was added, and heating was continued for an additional hour. The mixture was cooled and the solid was collected, washed with cold xylene, petroleum ether, dried, triturated with water, and dried in vacuo at 70° to give the product (24.7 g) as a yellow solid, mp 177°-179°.

후처리

  1. temperatureThe mixture was heated for one hour at 70°
  2. temperatureheating
  3. waitwas continued for an additional hour
  4. temperatureThe mixture was cooled
  5. customthe solid was collected
  6. washwashed with cold xylene, petroleum ether
  7. customdried
  8. customtriturated with water
  9. customdried in vacuo at 70°

출처 및 근거

ORD 기록
ord-5da7bd0770b34a0f955ea7401c71917a
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04582851

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