Sulfuric Acid → 4-Phenyl-2-nitrobenzenediazonium hydrogen sulfate

HRID 480510

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HRID 480510 반응식
[S:1](=[O:5])(=[O:4])([OH:3])[OH:2].[N:6]([O-])=O.[Na+].[N+:10]([C:13]1[CH:14]=[C:15]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:16]=[CH:17][C:18]=1[NH2:19])([O-:12])=[O:11].C(OCC)C>C(O)(=O)C>[S:1]([O-:5])([OH:4])(=[O:3])=[O:2].[C:20]1([C:15]2[CH:16]=[CH:17][C:18]([N+:19]#[N:6])=[C:13]([N+:10]([O-:12])=[O:11])[CH:14]=2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 3283Diethyl EtherHCID 77705[1,1'-Biphenyl]-4-amine, 3-nitro-2회HCID 23668193Sodium Nitrite2회

생성물 1

HCID 858226914-Phenyl-2-nitrobenzenediazonium hydrogen sulfate

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
20 °C

실험 절차

To 70 mL of sulfuric acid at 10° C. is added portionwise sodium nitrite (7 g, 0.1 mol). The reaction mixture is warmed to 20° C. to dissolve all the sodium nitrite and then cooled to 15° C. To the reaction mixture is added over 30 minutes a suspension of 3-nitro-4-amino-1,1′-biphenyl (7.33 g, 0.034 mol), prepared in (B) above, in 60 mL of acetic acid. The reaction mixture is stirred for one hour at 10° C. and then to the reaction mixture is added 500 mL of diethyl ether. An exotherm occurs. The mixture is stirred for one hour. The solid-formed is removed by filtration behind a safety shield and washed with diethyl ether to give 16.2 g of the title compound as a yellow solid. The solidis dried for 1.5 hours at 20° C. under vacuum and stored in a freezer in a polyethylene container until later use.

후처리

  1. temperaturecooled to 15° C
  2. additionTo the reaction mixture is added over 30 minutes
  3. stirringThe mixture is stirred for one hour
  4. customThe solid-formed is removed by filtration behind a safety shield
  5. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-f7addc823ac141eea820726b0f0a9c13
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06649770B1

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