1,2-Dichloroethane → 2-(4-Bromo-3,5-dimethyl-1H-pyrazol-1-yl)-1-(3-hydroxy-1-azetidinyl)ethanone

HRID 58066ノート

反応式

HRID 58066 の反応式
[Br:1][C:2]1[C:3]([CH3:12])=[N:4][N:5]([CH2:8][C:9]([OH:11])=O)[C:6]=1[CH3:7].[NH:13]1[CH2:16][CH:15]([OH:17])[CH2:14]1.C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl.C(N(C(C)C)C(C)C)C>CN(C=O)C.CCOC(C)=O>[Br:1][C:2]1[C:3]([CH3:12])=[N:4][N:5]([CH2:8][C:9]([N:13]2[CH2:16][CH:15]([OH:17])[CH2:14]2)=[O:11])[C:6]=1[CH3:7]

参加物

8

反応物 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 8196162-(4-bromo-3,5-dimethyl-1H-pyrazol-1-yl)acetic acidHCID 15142903-Hydroxyazetidine

生成物 1

HCID 897829192-(4-Bromo-3,5-dimethyl-1H-pyrazol-1-yl)-1-(3-hydroxy-1-azetidinyl)ethanone

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To 2-(4-bromo-3,5-dimethyl-1H-pyrazol-1-yl)acetic acid (0.4 g, 1.716 mmol) in DMF (6 mL) were added azetidin-3-ol (0.151 g, 2.060 mmol), HOBt (0.301 g, 2.231 mmol), and EDC (0.461 g, 2.403 mmol), followed by N-ethyl-N-isopropylpropan-2-amine (1.495 mL, 8.58 mmol). The reaction mixture was stirred for 18 hours at room temperature. The crude reaction mixture was subsequently diluted with EtOAc, washed with brine, dried over Na2SO4, and concentrated to give the title compound, which was used without further purification.

後処理

  1. customThe crude reaction mixture
  2. washwashed with brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-50b2cd0b08494a209af383aea6476a4e
出典データセット
uspto-grants-2016_09
特許番号
US09434743B2

反応ノート

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