Phenol → HCID 90449307、化合物

HRID 2274165ノート

反応式

HRID 2274165 の反応式
[CH2:1]([O:8][C:9]1[N:14]=[C:13](Cl)[N:12]=[C:11]([O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:23]1([OH:29])[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.C(N(CC)C(C)C)(C)C>ClCCl>[CH2:1]([O:8][C:9]1[N:14]=[C:13]([O:29][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[N:12]=[C:11]([O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 996PhenolHCID 81531DiisopropylethylamineHCID 90449221HCID 90449221、化合物

生成物 1

HCID 90449307HCID 90449307、化合物収率 99%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Next, a synthesis method of the hydroxy group-protecting agent 2 will be explained. To a 30 mL eggplant flask, 470.6 mg (1.50 m mol) of 6-benzyloxy-2-chloro-4-phenoxy-1,3,5-triazine, 3.00 mL of dichloromethane, 178.8 mg (1.90 m mol) of phenol and 0.390 mL (1.90 m mol) of N,N-diisopropylethylamine were added, and reacted at 0 degree under a nitrogen atmosphere for 4 hours. After the reaction, 50 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 to obtain 548.5 mg of 6-benzyloxy-2,4-diphenoxy-1,3,5-triazine (yield: 99%).

後処理

  1. customreacted at 0 degree under a nitrogen atmosphere for 4 hours
  2. additionwas added
  3. 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
  4. dry with materialA resulting organic phase was dried by magnesium sulfate, from which dichloromethane
  5. distillationwas distilled away

出典と根拠

ORDレコード
ord-426eeeb56c084bf782332413bb3cb9db
出典データセット
uspto-grants-2015_09
特許番号
US09126954B2

反応ノート

読み込み中…