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Ethyl Acetate → HCID 178510018, 화합물

HRID 1625209
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HRID 1625209 반응식
Br[C:2]1[CH:9]=[C:8]([N:10]2[C:14]3=[N:15][CH:16]=[CH:17][C:18]([C:19]4[CH:20]=[N:21][C:22]5[C:27]([CH:28]=4)=[CH:26][CH:25]=[CH:24][CH:23]=5)=[C:13]3[C:12]([C:29]([F:32])([F:31])[F:30])=[N:11]2)[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[OH:33][C@H:34]1[CH2:39][CH2:38][C@H:37]([NH2:40])[CH2:36][CH2:35]1.CC(C)([O-])C.[Na+].C(OCC)(=O)C>O1CCOCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.O>[OH:33][C@H:34]1[CH2:39][CH2:38][C@H:37]([NH:40][C:2]2[CH:9]=[C:8]([N:10]3[C:14]4=[N:15][CH:16]=[CH:17][C:18]([C:19]5[CH:20]=[N:21][C:22]6[C:27]([CH:28]=5)=[CH:26][CH:25]=[CH:24][CH:23]=6)=[C:13]4[C:12]([C:29]([F:32])([F:31])[F:30])=[N:11]3)[CH:7]=[CH:6][C:3]=2[C:4]#[N:5])[CH2:36][CH2:35]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8857Ethyl AcetateHCID 23676156Sodium t-butoxideHCID 67501770HCID 67501770, 화합물HCID 178511715HCID 178511715, 화합물

생성물 1

HCID 178510018HCID 178510018, 화합물수율 75.1%

시약·촉매·용매 3

HCID 167845palladium(II) acetate
촉매
HCID 962Water용매
HCID 312751,4-Dioxane용매

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온도
140 °C

실험 절차

A solution of a mixture of compound (1e) (0.560 g), trans-4-hydroxycyclohexylamine (0.522 g), sodium tert-butoxide (0.218 g), palladium acetate (0.025 g), and 1,1-bis-(diphenylphosphino)-ferrocene (0.126 g) in 1,4-dioxane (12 mL) was stirred under a nitrogen atmosphere at 140° C. for 2 hr. The reaction solution was distributed between ethyl acetate and water, and the organic layer was washed with saturated saline. The organic layer after the washing was dried over anhydrous sodium sulfate, and then the solvent was distilled away. The residue was purified by neutral silica gel column chromatography (chloroform/methanol) to obtain compound (1f) (0.450 g, 75%) as a white solid.

후처리

  1. washthe organic layer was washed with saturated saline
  2. dry with materialThe organic layer after the washing was dried over anhydrous sodium sulfate
  3. distillationthe solvent was distilled away
  4. customThe residue was purified by neutral silica gel column chromatography (chloroform/methanol)

출처 및 근거

ORD 기록
ord-2d602320785e4b16aa7153baf717d1bd
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08779142B2

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