Phenol → HCID 90449221, 화합물

HRID 2274164노트

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HRID 2274164 반응식
[CH2:1]([O:8][C:9]1[N:14]=[C:13](Cl)[N:12]=[C:11]([Cl:16])[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:17]1([OH:23])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C(N(CC)C(C)C)(C)C>ClCCl>[CH2:1]([O:8][C:9]1[N:10]=[C:11]([Cl:16])[N:12]=[C:13]([O:23][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 996PhenolHCID 356262-(Benzyloxy)-4,6-dichloro-1,3,5-triazineHCID 81531Diisopropylethylamine

생성물 1

HCID 90449221HCID 90449221, 화합물수율 94.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

Next, 5.70 mL of dichloromethane solution containing 896.2 mg (3.50 m mol) of 6-benzyloxy-2,4-dichloro-1,3,5-triazine, 2.00 mL of dichloromethane, 365.0 mg (3.88 m mol) of phenol and 0.738 mL (4.23 m mol) of N,N-diisopropylethylamine was added to a 30 mL eggplant flask, and reacted at 0 degree under a nitrogen atmosphere for 6 hours. After the reaction, 20 mL of dichloromethane was added, which was washed with 20 mL of 1 N hydrochloric acid, 20 mL of 1 N hydrochloric acid, 20 mL of water and 20 mL of saturated salt water. A resulting organic phase was dried by magnesium sulfate, from which dichloromethane was distilled away, and the residue was recrystallized to obtain 1033.2 mg of 6-benzyloxy-2-chloro-4-phenoxy-1,3,5-triazine (yield: 94%).

후처리

  1. additionwas added to a 30 mL eggplant flask
  2. customreacted at 0 degree under a nitrogen atmosphere for 6 hours
  3. additionwas added
  4. washwhich was washed with 20 mL of 1 N hydrochloric acid, 20 mL of 1 N hydrochloric acid, 20 mL of water and 20 mL of saturated salt water
  5. dry with materialA resulting organic phase was dried by magnesium sulfate, from which dichloromethane
  6. distillationwas distilled away
  7. customthe residue was recrystallized

출처 및 근거

ORD 기록
ord-899d01437bb84b039b7dc33f361d3b16
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126954B2

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