Hydrochloric Acid → 1,3-Benzenediol, 2-chloro-4,6-dinitro-

HRID 1609378노트

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HRID 1609378 반응식
[Cl:1][C:2]1[C:7](Cl)=[C:6]([N+:9]([O-:11])=[O:10])[CH:5]=[C:4]([N+:12]([O-:14])=[O:13])[C:3]=1[OH:15].CC(C)([O-:19])C.[K+].[OH-].[K+].Cl>O.CN1C(=O)CCC1>[Cl:1][C:2]1[C:7]([OH:19])=[C:6]([N+:9]([O-:11])=[O:10])[CH:5]=[C:4]([N+:12]([O-:14])=[O:13])[C:3]=1[OH:15]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 108579782,3-Dichloro-4,6-dinitrophenolHCID 23665647Potassium tert-butoxide

생성물 1

HCID 111072901,3-Benzenediol, 2-chloro-4,6-dinitro-수율 95%

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

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온도
85 °C

실험 절차

A solution of 2,3-dichloro-4,6-dinitrophenol (2.2 g, 0,008 mol, from previous example), 4.5 g of potassium t-butoxide, 0.4 g of potassium hydroxide, 30 mL of N-methyl pyrrolidinone, and 15 mL of water in a 100 mL round-bottomed flask with stir bar is heated to 85° C. for 6 hours. Upon completion, the reaction mixture is poured into 50 mL of aqueous hydrochloric acid. The resulting product is isolated by filtration, washed with cold water, and air dried. The product is recrystallized from a minimal amount of methanol to yield 1.97 g of 2-chloro-4,6-dinitroresorcinol (95% yield) (85% overall from 1,2-dichloro-3,5-dinitrobenzene).

후처리

  1. customThe resulting product is isolated by filtration
  2. washwashed with cold water, and air
  3. customdried
  4. customThe product is recrystallized from a minimal amount of methanol

출처 및 근거

ORD 기록
ord-5b3d6a07582e4fee91bc8002b06e4fc7
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05399768

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