Sodium Hydroxide → HCID 20308268, 화합물

HRID 1763885노트

반응식

HRID 1763885 반응식
[ClH:1].[CH3:2][N:3]([CH2:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[C:13]([Br:18])[CH:12]=1)[CH:4]1[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1.ClCl.[OH-].[Na+]>C(O)(=O)C>[CH3:2][N:3]([CH2:10][C:11]1[CH:16]=[C:15]([Cl:1])[C:14]([OH:17])=[C:13]([Br:18])[CH:12]=1)[CH:4]1[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9]1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24526ChlorineHCID 20308207HCID 20308207, 화합물

생성물 1

HCID 20308268HCID 20308268, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

3.6 gm of N-methyl-N-cyclohexyl-3-bromo-4-hydroxy-benzylamine hydrochloride were dissolved in 50 ml of 90% acetic acid and admixed with a solution of 0.85 gm of chlorine in 15 ml of glacial acetic acid while cooling with ice water. After stirring for a short time, the solution was poured into a mixture of ice and 10 N sodium hydroxide solution and extracted three times with methylene chloride. The organic phase was evaporated to dryness. The residue was purified by means of column chromatography over silicgel with ethyl acetate as the eluant, yielding N-methyl-N-cyclohexyl-3-bromo-5-chloro-4-hydroxy-benzylamine, m.p. 136°-138° C., of the formula ##STR24## after recrystallization from ethanol/ether.

후처리

  1. extractionextracted three times with methylene chloride
  2. customThe organic phase was evaporated to dryness
  3. customThe residue was purified by means of column chromatography over silicgel with ethyl acetate as the eluant

출처 및 근거

ORD 기록
ord-94a049545acc4aa183af8de752553c63
출처 데이터셋
uspto-grants-1978_09
특허 번호
US04113777

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