Diethyl Ether → HCID 58909953, 화합물

HRID 1295956노트

반응식

HRID 1295956 반응식
[C:1]([C:5]1[CH:6]=[C:7]([C:19](=[O:21])[CH3:20])[CH:8]=[C:9]([N:13]2[CH2:18][CH2:17][O:16][CH2:15][CH2:14]2)[C:10]=1[O:11][CH3:12])([CH3:4])([CH3:3])[CH3:2].[Cl:22]N1C(=O)CCC1=O.CCOCC>O1CCCC1.C(N(CC)CC)C>[Cl:22][CH2:20][C:19]([C:7]1[CH:8]=[C:9]([N:13]2[CH2:14][CH2:15][O:16][CH2:17][CH2:18]2)[C:10]([O:11][CH3:12])=[C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[CH:6]=1)=[O:21]

참가 물질

6

반응물 3

HCID 3283Diethyl EtherHCID 31398ChlorosuccinimideHCID 22929663HCID 22929663, 화합물

생성물 1

HCID 58909953HCID 58909953, 화합물수율 45.8%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8471Triethylamine용매

실험 절차

After dissolving 1-[3-(tert-butyl)-4-methoxy-5-morpholinophenyl]-1-ethanone (9.5 g) in tetrahydrofuran (60 ml), triethylamine (13 ml) and tert-butyl dimethylsilyltrifluoromethanesulfonate (9.8 ml) were added dropwise while cooling on ice. The reaction mixture was stirred for 30 minutes while cooling on ice and then N-chlorosuccinimide (5.3 g) was gradually added. After continuing to stir the reaction mixture for 30 minutes, ether (2 l) was added thereto and the resulting mixture was washed twice with water. The organic layer was dried over anhydrous magnesium sulfate and then the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (4.87 g) as light yellow crystals.

후처리

  1. additionwere added dropwise
  2. temperaturewhile cooling on ice
  3. temperaturewhile cooling on ice
  4. stirringto stir the reaction mixture for 30 minutes
  5. washthe resulting mixture was washed twice with water
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. customthe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)

출처 및 근거

ORD 기록
ord-b391e01203fa4787bf8428e36568c91d
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244730B2

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