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

HRID 449450노트

반응식

HRID 449450 반응식
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]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 59496759HCID 59496759, 화합물

생성물 1

HCID 553036832-(1-cyanocyclobutyl)acetic acid

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dce65a5a014e4e76a647fecd26aebc7a
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481732B2

반응 노트

불러오는 중…