2,4-Dichlorobenzyl chloride → HCID 69989841, 화합물

HRID 1358594노트

반응식

HRID 1358594 반응식
[CH3:1][O:2][C:3](=[O:19])[C@H:4]([CH2:13][C:14]1[N:18]=[CH:17][NH:16][CH:15]=1)[NH:5][C:6]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7].[Cl:20][C:21]1[CH:28]=[C:27]([Cl:29])[CH:26]=[CH:25][C:22]=1[CH2:23]Cl.CCN(CC)CC>C1C=CC=CC=1>[CH3:1][O:2][C:3](=[O:19])[C@H:4]([CH2:13][C:14]1[N:18]=[CH:17][N:16]([CH2:23][C:22]2[CH:25]=[CH:26][C:27]([Cl:29])=[CH:28][C:21]=2[Cl:20])[CH:15]=1)[NH:5][C:6]([O:8][C:9]([CH3:12])([CH3:10])[CH3:11])=[O:7]

참가 물질

5

반응물 3

HCID 72122,4-Dichlorobenzyl chlorideHCID 8471TriethylamineHCID 178501431HCID 178501431, 화합물

생성물 1

HCID 69989841HCID 69989841, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

N-(tert-butoxycarbonyl)-L-histidine methyl ester (1.0 g) was added to a solution of 2,4-dichlorobenzyl chloride (0.73 g) and Et3N (0.27 g) in benzene (10 ml) and the mixture was heated under reflux for 1 hr. The mixture was cooled and the precipitate was removed by filtration. The filtrate was washed with H2O, dried over Na2SO4, and the solvent was removed in vacuo. The residue was purified by column chromatography on silica gel (eluent; 95:5, CHCl3/MeOH) to give N-(tert-butoxycarbonyl)-1-[(2,4-dichlorophenyl)methyl]-L-histidine methyl ester. The obtained compound was treated in a similar manner as described in R. Example 4 to give 1-[(2,4-Dichlorophenyl)methyl]-L-histidine methyl ester, dihydrochloride salt.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1 hr
  3. temperatureThe mixture was cooled
  4. customthe precipitate was removed by filtration
  5. washThe filtrate was washed with H2O
  6. dry with materialdried over Na2SO4
  7. customthe solvent was removed in vacuo
  8. customThe residue was purified by column chromatography on silica gel (eluent; 95:5, CHCl3/MeOH)

출처 및 근거

ORD 기록
ord-bffab852faf34ffb8b40c06b1f428474
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06596752B1

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