Water → methyl N-methoxymethyl-N-(3-phenylbenzyl)carbamate

HRID 1168031노트

반응식

HRID 1168031 반응식
[C:1]1([C:7]2[CH:8]=[C:9]([CH:16]=[CH:17][CH:18]=2)[CH2:10][NH:11][C:12](=[O:15])[O:13][CH3:14])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Na+].[CH3:21][O:22][CH2:23]Br.O>O1CCCC1>[CH3:21][O:22][CH2:23][N:11]([CH2:10][C:9]1[CH:16]=[CH:17][CH:18]=[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH:8]=1)[C:12](=[O:15])[O:13][CH3:14]

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 83093Bromomethyl methyl etherHCID 12090300methyl N-(3-phenylbenzyl)carbamate

생성물 1

HCID 12090306methyl N-methoxymethyl-N-(3-phenylbenzyl)carbamate수율 76.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1.00 g of methyl N-(3-phenylbenzyl)carbamate in tetrahydrofuran (20 ml) was stirred together with 0.22 g of 60% sodium hydride at room temperature for 30 minutes. 0.78 g of methoxymethyl bromide was added dropwise at room temperature, and the resulting solution was stirred overnight. After the reaction, the reaction solution was poured into water and extracted with ethyl acetate, and the organic layer was separated, dried over anhydrous magnesium sulfate and evaporated under reduced pressure for removal of the solvent. The residue was purified by silica gel column chromatography to give 0.90 g of methyl N-methoxymethyl-N-(3-phenylbenzyl)carbamate as a pale yellow transparent viscous liquid.

후처리

  1. customAfter the reaction
  2. extractionextracted with ethyl acetate
  3. customthe organic layer was separated
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated under reduced pressure for removal of the solvent
  6. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-a241719dc28248dcb5e7c404b29c52ec
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06620961B1

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