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Isobutyl nitrite → Methyl 2-(4-(4-((4-chlorophenethyl)carbamoyl)phenoxy)-3-chlorophenyl)acetate

HRID 1927731
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인쇄 미리보기

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HRID 1927731 반응식
N(OCC(C)C)=O.[Cl:8][C:9]1[CH:39]=[CH:38][C:12]([CH2:13][CH2:14][NH:15][C:16]([C:18]2[CH:36]=[CH:35][C:21]([O:22][C:23]3[CH:28]=[CH:27][C:26]([CH2:29][C:30]([O:32][CH3:33])=[O:31])=[CH:25][C:24]=3[Cl:34])=[C:20](N)[CH:19]=2)=[O:17])=[CH:11][CH:10]=1>CN(C=O)C.C(OCC)(=O)C>[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:13][CH2:14][NH:15][C:16]([C:18]2[CH:36]=[CH:35][C:21]([O:22][C:23]3[CH:28]=[CH:27][C:26]([CH2:29][C:30]([O:32][CH3:33])=[O:31])=[CH:25][C:24]=3[Cl:34])=[CH:20][CH:19]=2)=[O:17])=[CH:38][CH:39]=1
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참가 물질

5

반응물 2

HCID 10958Isobutyl nitriteHCID 68467172Methyl 2-(4-(4-((4-chlorophenethyl)carbamoyl)-2-aminophenoxy)-3-chlorophenyl)acetate

생성물 1

HCID 68466220Methyl 2-(4-(4-((4-chlorophenethyl)carbamoyl)phenoxy)-3-chlorophenyl)acetate수율 72.4%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 8857Ethyl Acetate
용매

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온도
60 °C

실험 절차

Isobutyl nitrite (0.0751 ml, 0.634 mmol) was diluted with DMF (1 mL), placed under nitrogen and heated to 60° C. Methyl 2-(4-(4-((4-chlorophenethyl)carbamoyl)-2-aminophenoxy)-3-chlorophenyl)acetate (100 mg, 0.211 mmol) in DMF (1 mL) was added dropwise and the reaction was stirred for 1 hour. The reaction was cooled, diluted with ethyl acetate and washed with 2N HCl, saturated sodium bicarbonate and brine. The organic layer was dried over MgSO4, filtered and concentrated. The material was purified using a biotage 12i column, eluting with DCM:MeOH (99:1) to yield methyl 2-(4-(4-((4-chlorophenethyl)carbamoyl)phenoxy)-3-chlorophenyl)acetate (70 mg, 72.3% yield).

후처리

  1. temperatureThe reaction was cooled
  2. washwashed with 2N HCl, saturated sodium bicarbonate and brine
  3. dry with materialThe organic layer was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe material was purified
  7. washeluting with DCM:MeOH (99:1)

출처 및 근거

ORD 기록
ord-930983b26de04890a31a4bd6af2cfe98
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08183289B2

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