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Methyl chloroformate → HCID 59831668, 화합물

HRID 268749
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HRID 268749 반응식
[NH:1]1[C:9]2[C:4](=[C:5]([CH:10]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:11][CH2:12][NH2:13])[CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.Cl[C:21]([O:23][CH3:24])=[O:22]>C(Cl)Cl>[CH3:24][O:23][C:21](=[O:22])[NH:13][CH2:12][CH2:11][CH:10]([C:5]1[CH:6]=[CH:7][CH:8]=[C:9]2[C:4]=1[CH:3]=[CH:2][NH:1]2)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1
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참가 물질

4

반응물 2

HCID 6586Methyl chloroformateHCID 25261580HCID 25261580, 화합물

생성물 1

HCID 59831668HCID 59831668, 화합물수율 98%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

To a stirring solution of 3-(1H-indol-4-yl)-3-phenyl-propylamine (III) (0.40 g, 1.6 mmol) in DCM (15 ml), under N2, was added TEA (0.23 ml, 1.7 mmol). The mixture was cooled to about 0° C. and methyl chloroformate (0.13 ml, 1.7 mmol) in DCM (10 ml) was added dropwise over 15 minutes. The mixture was stirred at room temperature for 30 minutes, quenched by addition of H2O, and stirred for 10 min. The mixture was washed successively with H2O and brine, dried over Na2SO4, filtered, and concentrated in vacuo to provide [3-(1H-indol-4-yl)-3-phenyl-propyl]-carbamic acid methylester (V) as a white solid (0.48 g, 98% yield).

후처리

  1. customquenched by addition of H2O
  2. stirringstirred for 10 min
  3. washThe mixture was washed successively with H2O and brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-c6ed860f74c749099383eb738808e059
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07446118B2

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