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Pyridine → Butanoic acid, 4-chloro-, 1,1-dimethylethyl ester

HRID 412705
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HRID 412705 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5](Cl)=[O:6].N1C=CC=CC=1.[C:14]([OH:18])([CH3:17])([CH3:16])[CH3:15]>CN(C)C1C=CN=CC=1>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([O:18][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 6386tert-ButanolHCID 783704-Chlorobutyryl chloride

생성물 1

HCID 527695Butanoic acid, 4-chloro-, 1,1-dimethylethyl ester수율 73%

시약·촉매·용매 1

HCID 142844-(Dimethylamino)pyridine촉매

실험 절차

A mixture comprising 4-chlorobutyryl chloride (12.6 g, 89.2 mmol), tert-butanol (25 mL), pyridine (6.9 g, 86.5 mmol) and 4-dimethylaminopyridine (1.0 g, 8.2 mmol) was heated at 50° C. under an atmosphere of dry nitrogen for 12 hours to give a white suspension. The suspension was partitioned between ethyl ether (250 mL) and water and the organic layer was separated and washed repeatedly with water then 0.1M aqueous hydrochloric acid, saturated aqueous sodium carbonate and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to a colorless oil. The oil was distilled at 0.5 mmHg (51° C.) to provide tert-butyl 4-chlorobutyrate as a colorless liquid (11.27 g, 73% yield); 1H NMR (300 MHz, CDCl3): 3.60 (tr, 2H), 2.40 (tr, 2H), 2.10 (m, 2H), 1.45 (s, 9H).

후처리

  1. customto give a white suspension
  2. customThe suspension was partitioned between ethyl ether (250 mL) and water
  3. customthe organic layer was separated
  4. washwashed repeatedly with water
  5. dry with material0.1M aqueous hydrochloric acid, saturated aqueous sodium carbonate and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo to a colorless oil
  8. distillationThe oil was distilled at 0.5 mmHg (51° C.)

출처 및 근거

ORD 기록
ord-3b4df59348ff4b0e9f721208572e0d23
출처 데이터셋
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06562854B2

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