Hydrochloric Acid → 5-n-Butylthio-2-(2-hydroxy-3,5-di-tert-butylphenyl)-2H-benzotnazole

HRID 1276856노트

반응식

HRID 1276856 반응식
Cl[C:2]1[CH:25]=[CH:24][C:5]2=[N:6][N:7]([C:9]3[CH:14]=[C:13]([C:15]([CH3:18])([CH3:17])[CH3:16])[CH:12]=[C:11]([C:19]([CH3:22])([CH3:21])[CH3:20])[C:10]=3[OH:23])[N:8]=[C:4]2[CH:3]=1.[CH2:26]([SH:30])[CH2:27][CH2:28][CH3:29].[OH-].[K+].CN1CCCC1=O.Cl>>[CH2:26]([S:30][C:2]1[CH:25]=[CH:24][C:5]2=[N:6][N:7]([C:9]3[CH:14]=[C:13]([C:15]([CH3:18])([CH3:17])[CH3:16])[CH:12]=[C:11]([C:19]([CH3:22])([CH3:21])[CH3:20])[C:10]=3[OH:23])[N:8]=[C:4]2[CH:3]=1)[CH2:27][CH2:28][CH3:29]

참가 물질

6

반응물 5

HCID 313Hydrochloric AcidHCID 8012ButanethiolHCID 13387N-methyl-2-pyrrolidoneHCID 14797Potassium HydroxideHCID 774702,4-Di-tert-butyl-6-(5-chloro-2H-benzotriazol-2-yl)phenol

생성물 1

HCID 186728395-n-Butylthio-2-(2-hydroxy-3,5-di-tert-butylphenyl)-2H-benzotnazole

반응 조건

온도
150 °C

실험 절차

5-Chloro-2-(2-hydroxy-3,5-di-tert-butylphenyl)-2H-benzotriazole (21.2 g, 0.06 mol), n-butyl mercaptan (7.2 g, 0.08 mol), potassium hydroxide (6.7.1 g, 0.12 mol) and N-methylpyrrolidone (50 g, 0.5 mol) are charged to a reactor and heated to 150° C. The reaction mass is held at 150° C. for 4.5 hours at which time it then cooled to ambient temperature. A mixture of 15 g of concentrated hydrochloric acid aand 70 g of ice are then added to the reactor. The solids are filtered off and washed with water. Thirty gram of crude, wet, yellow crystals are obtained as the title compound. This product can be used "as is" in procedure of Example 33.

후처리

  1. temperaturethen cooled to ambient temperature
  2. additionare then added to the reactor
  3. filtrationThe solids are filtered off
  4. washwashed with water

출처 및 근거

ORD 기록
ord-2973f08c0edd4bbfb5a1af277316b527
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06166218

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