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

HRID 1879603

反応式

HRID 1879603 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

反応条件

温度
110 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6b98eb3eef874f4598a57fcbdcc3693e
出典データセット
uspto-grants-2012_11
特許番号
US08318133B2

関連ノート

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