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Water → 1-(5-Nitropyridin-2-yl)azetidin-3-ol

HRID 1019542
ノート
印刷プレビュー

反応式

HRID 1019542 の反応式
Cl.[OH:2][CH:3]1[CH2:6][NH:5][CH2:4]1.Cl[C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][N:9]=1.C(N(CC)CC)C.O>CN(C)C=O.C(OCC)(=O)C>[OH:2][CH:3]1[CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][N:9]=2)[CH2:4]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 783082-Chloro-5-nitropyridineHCID 27592903-Hydroxyazetidine hydrochloride

生成物 1

HCID 529372641-(5-Nitropyridin-2-yl)azetidin-3-ol

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
100 °C

実験手順

A mixture of 0.311 g (2.84 mmol) of 3-hydroxyazetidine hydrochloride, 0.3 g (1.89 mmol) of 2-chloro-5-nitropyridine and 0.41 mL (2.84 mmol) of triethylamine in 10 mL of dimethylformamide is heated overnight at 100° C. After this time, the suspension is poured into a mixture of 30 mL of water and 30 mL of ethyl acetate. The aqueous phase is separated, and then extracted with 20 mL of ethyl acetate. The organic phases are combined, washed three times with 25 mL of water, then dried over sodium sulfate and concentrated at reduced pressure. We thus obtain 0.34 g of the expected product in the form of a solid, which will be used as it is in the rest of the synthesis.

後処理

  1. customThe aqueous phase is separated
  2. extractionextracted with 20 mL of ethyl acetate
  3. washwashed three times with 25 mL of water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated at reduced pressure
  6. customis in the rest of the synthesis

出典と根拠

ORDレコード
ord-3bdfce21be3f487086618c3444a71143
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08716272B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート