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

HRID 2262449

反応式

HRID 2262449 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

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. filtrationthe precipitated was collected by filtration
  3. customtriturated with DCM thoroughly
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-e224e825d3ac45ae80c1cdf8b7c8f606
出典データセット
uspto-grants-2010_12
特許番号
US07850946B2

関連ノート

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