Hydrochloric Acid → 2-(2H-Benzotriazol-2-yl)-4,6-bis(1-methyl-1-phenylethyl)phenol

HRID 1680614ノート

反応式

HRID 1680614 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]=[N:11][C:12]1[CH:17]=[C:16]([C:18]([CH3:26])([CH3:25])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:15]=[C:14]([C:27]([CH3:35])([CH3:34])[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:13]=1[OH:36])([O-])=O.C1(C)C=CC=CC=1.[OH-].[Na+].Cl>[Zn].O.C(O)(C)C>[OH:36][C:13]1[C:14]([C:27]([CH3:35])([CH3:34])[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)=[CH:15][C:16]([C:18]([CH3:26])([CH3:25])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[CH:17][C:12]=1[N:11]1[N:10]=[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]2=[N:1]1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 1140TolueneHCID 14798Sodium HydroxideHCID 1168102,4-Bis(1-methyl-1-phenylethyl)-6-[2-(2-nitrophenyl)diazenyl]phenol

生成物 1

HCID 1124122-(2H-Benzotriazol-2-yl)-4,6-bis(1-methyl-1-phenylethyl)phenol

試薬・触媒・溶媒 3

HCID 23994Zinc触媒4 回HCID 962Water溶媒HCID 3776Isopropanol溶媒

反応条件

温度
40 °C

実験手順

To a 5-liter 3-necked flask fitted with a stirrer, thermometer, reflux condenser and nitrogen inlet was charged 386 grams (0.805 mol) of the o-nitroazobenzene intermediate of Example 2 and 1200 ml of toluene. To the resulting solution was added 240 ml of isopropanol and 240 ml of water. A nitrogen atmosphere was imposed and 160 ml of 50.15 aqueous sodium hydroxide was added. A flask containing 158.2 grams (2.42 gram-atoms) of zinc was connected to the reaction flask by Gooch rubber tubing and the zinc dust was added portionwise to the reaction mixture over a 90-minute period. The zinc was added at such a rate to keep the internal temperature between 40° and 45° C. After the zinc was all added, the reaction mixture was heated for 1 hour at 40° C. and then for 3 hours at 70° C. The mixture was cooled to room temperature and acidified with 600 ml of concentrated hydrochloric acid.

後処理

  1. customTo a 5-liter 3-necked flask fitted with a stirrer
  2. temperaturethermometer, reflux condenser and nitrogen inlet
  3. customthe internal temperature between 40° and 45° C
  4. temperatureThe mixture was cooled to room temperature

出典と根拠

ORDレコード
ord-ff220221845e425989c9b5d57f14220d
出典データセット
uspto-grants-1981_06
特許番号
US04275004

反応ノート

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