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Acetic Acid → HCID 44243038, 화합물

HRID 1013090
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HRID 1013090 반응식
OC(C(F)(F)F)=O.[NH2:8][C:9]1([C:32]([NH2:34])=[O:33])[CH2:14][CH2:13][N:12]([C:15]([C:17]2[C:18]3[CH:31]=[CH:30][CH:29]=[CH:28][C:19]=3[S:20][C:21]=2[NH:22][C:23]([NH:25][CH2:26][CH3:27])=[O:24])=[O:16])[CH2:11][CH2:10]1.C(O)(=O)C.[CH2:39]([O:41][C:42](OCC)([O:50]CC)[CH2:43][CH2:44][C:45](OCC)=O)[CH3:40]>C1(C)C=CC=CC=1.CN(C=O)C>[CH2:26]([NH:25][C:23](=[O:24])[NH:22][C:21]1[S:20][C:19]2[CH:28]=[CH:29][CH:30]=[CH:31][C:18]=2[C:17]=1[C:15]([N:12]1[CH2:11][CH2:10][C:9]2([N:8]=[C:45]([CH2:44][CH2:43][C:42]([O:41][CH2:39][CH3:40])=[O:50])[NH:34][C:32]2=[O:33])[CH2:14][CH2:13]1)=[O:16])[CH3:27]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 13452377Ethyl 4,4,4-triethoxybutanoateHCID 44243036HCID 44243036, 화합물

생성물 1

HCID 44243038HCID 44243038, 화합물수율 65%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6228Dimethylformamide용매

반응 조건

온도
85 °C

실험 절차

4-Amino-1-(2-(3-ethylureido)benzo[b]thiophene-3-carbonyl)piperidine-4-carboxamide (7, 100 mg, 1.0 equivalent) as prepared in Example 7 was dissolved in toluene (0.09 M) and DMF (0.26 M), and to which acetic acid (2.0 equivalents), and ethyl 4,4,4-triethoxybutanoate (4.0 equivalents) were added and the reaction mixture was heated to 85° C. for 9 hrs. The reaction mixture was then partitioned between ethyl acetate and water and the separated organics was washed with brine and dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by SiO2 chromatography (5%-10% MeOH/CH2Cl2 gradient) to afford ethyl 3-(8-(2-(3-ethylureido)benzo[b]thiophene-3-carbonyl)-4-oxo-1,3,8-triazaspiro[4.5]dec-1-en-2-yl)propanoate (10, 65%). Two rotamers observed (ratio 1.3:1).

후처리

  1. customThe reaction mixture was then partitioned between ethyl acetate and water
  2. washthe separated organics was washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by SiO2 chromatography (5%-10% MeOH/CH2Cl2 gradient)

출처 및 근거

ORD 기록
ord-5c8e6aa685ce424e95a19a6b0660754c
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981904B2

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