3-Bromopropionic acid → 1,1,2-trimethyl[1H]-benz[e]indole-3-propanoic acid

HRID 1879603

반응식

HRID 1879603 반응식
[CH3:1][C:2]1([CH3:16])[C:10]2[C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[CH:7]=[CH:6][C:5]=2[N:4]=[C:3]1[CH3:15].Br[CH2:18][CH2:19][C:20]([OH:22])=[O:21]>ClC1C=CC=CC=1Cl>[CH3:1][C:2]1([CH3:16])[C:10]2[C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[CH:7]=[CH:6][C:5]=2[N:4]([CH2:18][CH2:19][C:20]([OH:22])=[O:21])[CH:3]1[CH3:15]

참가 물질

4

반응물 2

HCID 115533-Bromopropionic acidHCID 1705302,3,3-Trimethylbenzoindolenine

생성물 1

HCID 669869251,1,2-trimethyl[1H]-benz[e]indole-3-propanoic acid수율 112.2%

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

반응 조건

온도
110 °C

실험 절차

A mixture of 1,1,2-trimethyl[1H]-benz[e]indole (10.0 g, 47.8 mmol) and 3-bromopropanoic acid (7.3 g, 47.8 mmol) in 1,2-dichlorobenzene (50 mL) was heated with stirring at 110° C. for 18 h. After the resulting mixture was cooled to room temperature, the precipitated was collected by filtration, triturated with DCM thoroughly, and dried under vacuum to afford 15.2 g of light brown powder (88%). ESI-MS: observed for [MH]+281.31.

후처리

  1. temperaturewas heated
  2. temperatureAfter the resulting mixture was cooled to room temperature
  3. filtrationthe precipitated was collected by filtration
  4. customtriturated with DCM thoroughly
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-6b98eb3eef874f4598a57fcbdcc3693e
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318133B2

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