Dichloromethane → HCID 13064229, 화합물

HRID 894226노트

반응식

HRID 894226 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1)#[N:2].Cl[CH2:11][C:12]1[CH:17]=[C:16]([F:18])[CH:15]=[C:14]([CH2:19]Cl)[C:13]=1[OH:21].[Cl-].[Al+3].[Cl-].[Cl-].ClCCl>[N+](C1C=CC=CC=1)([O-])=O>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([OH:9])=[C:7]([CH:8]=1)[CH2:11][C:12]1[CH:17]=[C:16]([F:18])[CH:15]=[C:14]([CH2:19][C:5]2[CH:4]=[C:3]([C:1]#[N:2])[CH:8]=[CH:7][C:6]=2[OH:9])[C:13]=1[OH:21])#[N:2]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 130194-CyanophenolHCID 6451240Aluminum(III) ChlorideHCID 211628322,6-Bis(chloromethyl)-4-fluorophenol

생성물 1

HCID 13064229HCID 13064229, 화합물수율 3%

시약·촉매·용매 1

HCID 7416Nitrobenzene용매

실험 절차

p-Cyanophenol (19.4 g) and 2,6-bis(chloromethyl)-4-fluorophenol (17.0 g) were dissolved in nitrobenzene (250 ml) at 20°. The solution was cooled to 10° and crushed aluminium chloride (anhydrous 65 g) was added in 5 g portions over two hours. During the addition the temperature was maintained at 10°-12°. Stirring was continued at 20° for 14 hrs. The viscous black mixture was poured onto a vigorously stirred mixture of ice (2 l) and dichloro methane (2 l). The organic solvent layer was dried, dichloro methane and nitrobenzene removed by vacuum distillation and the residual tar passed through a silica column. The product, 2,6-bis(5-cyano-2-hydroxybenzyl)-4-fluorophenol (mp 222°) was obtained in 3% yield.

후처리

  1. temperatureThe solution was cooled to 10°
  2. additionwas added in 5 g portions over two hours
  3. additionDuring the addition the temperature
  4. temperaturewas maintained at 10°-12°
  5. customThe organic solvent layer was dried
  6. customdichloro methane and nitrobenzene removed by vacuum distillation

출처 및 근거

ORD 기록
ord-4112cdcdabda4ece86850fe58305beb4
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04282390

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