Hydrochloric Acid → 2-(1-cyanocyclobutyl)acetic acid

HRID 449450ノート

反応式

HRID 449450 の反応式
CC1(C)OC(=O)[CH:5]([C:9]2([C:13]#[N:14])[CH2:12][CH2:11][CH2:10]2)[C:4](=[O:15])[O:3]1.Cl>O>[C:13]([C:9]1([CH2:5][C:4]([OH:15])=[O:3])[CH2:12][CH2:11][CH2:10]1)#[N:14]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 59496759HCID 59496759、化合物

生成物 1

HCID 553036832-(1-cyanocyclobutyl)acetic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
100 °C

実験手順

The reaction mixture of 1-(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-yl)cyclobutanecarbonitrile (0.32 g, 1.4 mmol) in N,N-dimethylformate (4.0 mL) and water (0.40 mL) was stirred at 100° C. for 2 h. After cooled to r.t., the mixture was diluted with water, adjusted to pH=2 with aqueous HCl, and extracted with ethyl acetate (3×20 mL). The combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated under reduced pressure to afford the crude product which was directly used in next step reaction without further purification.

後処理

  1. temperatureAfter cooled to r.t.
  2. extractionextracted with ethyl acetate (3×20 mL)
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-dce65a5a014e4e76a647fecd26aebc7a
出典データセット
uspto-grants-2013_07
特許番号
US08481732B2

反応ノート

読み込み中…