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Triethylamine → HCID 59255129, 화합물

HRID 640406
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HRID 640406 반응식
[CH2:1]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C:12](Cl)=[N:13][OH:14])=[CH:7][CH:6]=1)[CH2:2][CH2:3][CH3:4].[C:16]([C:18]1[C:19]([NH2:25])=[N:20][C:21]([NH2:24])=[CH:22][CH:23]=1)#[CH:17].C(N(CC)CC)C>O1CCCC1>[CH2:1]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C:12]2[CH:17]=[C:16]([C:18]3[C:19]([NH2:25])=[N:20][C:21]([NH2:24])=[CH:22][CH:23]=3)[O:14][N:13]=2)=[CH:7][CH:6]=1)[CH2:2][CH2:3][CH3:4]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 552816763-Ethynylpyridine-2,6-diamineHCID 72262855(4-Butyl-phenyl)-acetohydroximoyl chloride

생성물 1

HCID 59255129HCID 59255129, 화합물수율 48.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a tetrahydrofuran (3 mL) solution of (4-butyl-phenyl)-acetohydroximoyl chloride (150 mg, 0.665 mmol) described in Manufacturing Example 70-1-3 and 3-ethynyl-pyridin-2,6-diamine (56.5 mg, 0.424 mmol) described in Manufacturing Example 13-1-3 was added triethylamine (232 μL, 1.66 mmol). This mixture was stirred for 5 hours at room temperature. The mixture was partitioned into ethyl acetate and water. The organic layer was separated, washed with water, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=1:1˜ethyl acetate) to obtain the title compound (66 mg, 31%).

후처리

  1. customThe mixture was partitioned into ethyl acetate and water
  2. customThe organic layer was separated
  3. washwashed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under a reduced pressure
  7. customthe residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=1:1˜ethyl acetate)

출처 및 근거

ORD 기록
ord-8e39db682e2a4a6fb12ebd70a1538143
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691882B2

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