Sodium Hydroxide → HCID 20308268, 화합물

HRID 616409노트

반응식

HRID 616409 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 0.75 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 silicagel 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 ##STR29## 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 silicagel with ethyl acetate as the eluant

출처 및 근거

ORD 기록
ord-2b1fa3159d4f4678b9f04cd7568d8557
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04073942

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