Sodium Chloride → HCID 12090302, 화합물

HRID 1168035

반응식

HRID 1168035 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

10.00 g of 3-bromobenzylamine hydrochloride suspended in chloroform (100 ml) was mixed with 9.55 g of triethylamine at room temperature. The resulting solution was stirred under cooling with ice while 4.67 g of methyl chloroformate was added dropwise and then stirred at room temperature for 2 hours. After the reaction, the reaction solution was poured into saturated aqueous sodium chloride, and the organic layer was separated, dried over anhydrous magnesium sulfate and evaporated at ordinary pressure for removal of the solvent. The residue was purified by silica gel column chromatography to give 9.54 g of methyl N-(3-bromobenzyl)carbamate as white crystals. m.p. 41-44° C.

후처리

  1. additionwas added dropwise
  2. stirringstirred at room temperature for 2 hours
  3. customAfter the reaction
  4. customthe organic layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated at ordinary pressure for removal of the solvent
  7. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-843bda6c90424b4391826737afe549f1
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06620961B1

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