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

HRID 1609378ノート

反応式

HRID 1609378 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
85 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-5b3d6a07582e4fee91bc8002b06e4fc7
出典データセット
uspto-grants-1995_03
特許番号
US05399768

反応ノート

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