Water → HCID 59639634、化合物

HRID 2357304ノート

反応式

HRID 2357304 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[N:9]1[C:14]2[N:15]=[C:16]([NH:27][CH2:28][C:29]([NH:31][CH2:32][CH2:33][O:34]C)=[O:30])[N:17]=[C:18]([C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:20]=3[CH3:26])[C:13]=2[CH:12]=[CH:11][C:10]1=[O:36].B(Br)(Br)Br.O>ClCCl>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[N:9]1[C:14]2[N:15]=[C:16]([NH:27][CH2:28][C:29]([NH:31][CH2:32][CH2:33][OH:34])=[O:30])[N:17]=[C:18]([C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:20]=3[CH3:26])[C:13]=2[CH:12]=[CH:11][C:10]1=[O:36]

参加物

5

反応物 3

HCID 962WaterHCID 25134Boron tribromideHCID 59639571HCID 59639571、化合物

生成物 1

HCID 59639634HCID 59639634、化合物収率 62.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a soln of the product of Example 205 (50 mg, 0.1 mmol), in dichloromethane (2 mL) was added 1 M boron tribromide in dichloromethane (0.5 mL, 0.5 mmol). The mixture was stirred at 23° for 2 h, H2O was added, extracted with EtOAc. The organic layer was dried (Na2SO4) and concentrated to give the crude material. Recrystallization from dichloromethane and hexane afforded the title product (30 mg, 62%). LC-MS: 484.2 (MH+, m/z), 1.59 (Rt, min).

後処理

  1. extractionextracted with EtOAc
  2. dry with materialThe organic layer was dried (Na2SO4)
  3. concentrationconcentrated
  4. customto give the crude material
  5. customRecrystallization from dichloromethane and hexane

出典と根拠

ORDレコード
ord-e806a11024704fb19dc65d2aba4fa9b8
出典データセット
uspto-grants-2010_07
特許番号
US07759486B2

反応ノート

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