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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Potassium Carbonate → Carbamic acid, (4-amino-2-methyl-5-nitrophenyl)-, 2-chloroethyl ester

HRID 980418
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HRID 980418 반응식
[CH3:1][C:2]1[CH:8]=[C:7]([NH2:9])[C:6]([N+:10]([O-:12])=[O:11])=[CH:5][C:3]=1[NH2:4].C(=O)([O-])[O-].[K+].[K+].O1CCOCC1.[Cl:25][CH2:26][CH2:27][O:28][C:29](Cl)=[O:30]>O>[CH3:1][C:2]1[CH:8]=[C:7]([NH2:9])[C:6]([N+:10]([O-:12])=[O:11])=[CH:5][C:3]=1[NH:4][C:29](=[O:30])[O:28][CH2:27][CH2:26][Cl:25]
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참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 123052-Chloroethyl chloroformateHCID 312751,4-DioxaneHCID 54879442-Methyl-5-nitrobenzene-1,4-diamine

생성물 1

HCID 14774569Carbamic acid, (4-amino-2-methyl-5-nitrophenyl)-, 2-chloroethyl ester

시약·촉매·용매 1

HCID 962Water
용매

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온도
90 °C

실험 절차

0.6 mol (100 g) of 2-methyl-4-amino-5-nitroaniline and 0.36 mol (50 g) of potassium carbonate are introduced into 500 ml of dioxane to which 145 ml of water have been added. The mixture is brought to 90° C., while stirring, and 0.6 mol (86 g) of chloroethylchloroformate is added a little at a time, in the course of 10 minutes. When the addition has ended, heating at 90° C. is continued for 10 minutes and the reaction mixture is cooled to 15° C. and the expected product is filtered off with suction. After being washed with a little dioxane and then with water and alcohol, the product is recrystallised from dioxane and then dried in vacuo. It has a melting point of 192° C.

후처리

  1. additionhave been added
  2. customis brought to 90° C.
  3. customin the course of 10 minutes
  4. additionWhen the addition
  5. temperaturethe reaction mixture is cooled to 15° C.
  6. filtrationthe expected product is filtered off with suction
  7. washAfter being washed with a little dioxane
  8. customwith water and alcohol, the product is recrystallised from dioxane
  9. customdried in vacuo

출처 및 근거

ORD 기록
ord-7265f95b274042d98f6baa66fcdd38b2
출처 데이터셋
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04637821

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