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Hydrochloric Acid → HCID 86631895, 화합물

HRID 1163475
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HRID 1163475 반응식
[N:1]1[N:2]([C:10]2[CH:15]=[C:14]([CH3:16])[CH:13]=[CH:12][C:11]=2[OH:17])[N:3]=[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12.[OH-].[K+].Br[CH:21]([CH3:39])[C:22]([C:24]1[CH:29]=[C:28]([C:30]([CH3:33])([CH3:32])[CH3:31])[C:27]([OH:34])=[C:26]([C:35]([CH3:38])([CH3:37])[CH3:36])[CH:25]=1)=[O:23].Cl>CN1CCCC1=O.O>[N:1]1[N:2]([C:10]2[CH:15]=[C:14]([CH3:16])[CH:13]=[CH:12][C:11]=2[O:17][CH:21]([CH3:39])[C:22]([C:24]2[CH:29]=[C:28]([C:30]([CH3:31])([CH3:33])[CH3:32])[C:27]([OH:34])=[C:26]([C:35]([CH3:38])([CH3:37])[CH3:36])[CH:25]=2)=[O:23])[N:3]=[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 17113DrometrizoleHCID 13173168HCID 13173168, 화합물

생성물 1

HCID 86631895HCID 86631895, 화합물수율 76.4%

시약·촉매·용매 2

HCID 962Water용매
HCID 13387
N-methyl-2-pyrrolidone
용매
2회

실험 절차

A mixture of 5.5 g (24 mmol) of 2-benzotriazol-2-yl-4-methyl-phenol, 4.7 g (72 mmol) of potassium hydroxide and 100 ml of n-methylpyrrolidone is stirred for 2 hours at room temperature. Then 8.0 g (24 mmol) 2-bromo-1-(3,5-di-tert-butyl-4-hydroxyphenyl)-propan-1-one dissolved in 40 ml of n-methylpyrrolidone is added and stirring is continued at room temperature for 20 hours. After the addition of 50 ml of water and 15 ml 2N hydrochloric acid the precipitated solid is filtered off and recrystallized from ethanol to give 8.9 g (76%) of compound 117; m.p. 161° C.

후처리

  1. additionis added
  2. stirringstirring
  3. waitis continued at room temperature for 20 hours
  4. filtrationis filtered off
  5. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-0a6d20fc30044925bb8571c3076ec39b
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07820865B2

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