Sodium Chloride → HCID 12090302, 화합물

HRID 427250

반응식

HRID 427250 반응식
Cl.[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH2:7].C(N(CC)CC)C.Cl[C:19]([O:21][CH3:22])=[O:20].[Cl-].[Na+]>C(Cl)(Cl)Cl>[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH:7][C:19](=[O:20])[O:21][CH3:22]

참가 물질

6

반응물 4

HCID 5234Sodium ChlorideHCID 6586Methyl chloroformateHCID 8471TriethylamineHCID 27249803-Bromobenzylamine hydrochloride

생성물 1

HCID 12090302HCID 12090302, 화합물수율 87%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a suspension of 10.0 g of 3-bromobenzylamine hydrochloride in chloroform (100 ml), 9.55 g of triethylamine was added at room temperature. To this solution, 4.67 g of methyl chloroformate was dropwise added under cooling with ice, followed by stirring at room temperature for 2 hours. The reaction solution was poured into a sodium chloride aqueous solution, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography to obtain 9.54 g of methyl N-(3-bromobenzyl)carbamate as white crystals.

후처리

  1. additionwas added at room temperature
  2. temperatureunder cooling with ice
  3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-2e7b3b0e1e124827b5f8cf77d7fe0b6a
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313071B1

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