Phenol → HCID 90449221、化合物

HRID 2274164ノート

反応式

HRID 2274164 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 90449221HCID 90449221、化合物収率 94.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-899d01437bb84b039b7dc33f361d3b16
出典データセット
uspto-grants-2015_09
特許番号
US09126954B2

反応ノート

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