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Pyridine → 1-Chloroethyl Hexyl Carbonate

HRID 745042
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HRID 745042 반응식
Cl[C:2]([O:4][CH:5]([Cl:7])[CH3:6])=[O:3].[CH2:8]([OH:14])[CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].N1C=CC=CC=1>C(Cl)(Cl)Cl>[C:2](=[O:3])([O:14][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[O:4][CH:5]([Cl:7])[CH3:6]
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참가 물질

5

반응물 3

HCID 1049PyridineHCID 81031-HexanolHCID 5213051-Chloroethyl chloroformate

생성물 1

HCID 135066371-Chloroethyl Hexyl Carbonate

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

1-Chloroethyl chloroformate (10.0 g, 69.9 mmol) and 1-hexanol (6.5 g, 63.6 mmol) were dissolved in chloroform (80 ml) at 0° C. Pyridine (5.5 g, 69.5 mmol) was added dropwise during 17 minutes maintaining the temperature below 10° C. After stirring at room temperature for 20 hours the organic phase was washed three times with 1 normal hydrochloric acid, once with a saturated sodium hydrogen carbonate solution and finally twice with water. The organic solution was dried with magnesium sulfate and the solvent was removed at reduced pressure. The residue (11.6 g) was distilled in vacuo (Bp. 61°-72° C., 3×10-3 mbar). Yield: 9.0 g. 1H-NMR (CDCl3): delta=0.89 (CH2CH3); 1.28-1.40 (CH2CH2CH×2CH3); 1.69 (OCH2CH2); 1.83 (CH3CH); 4.20 (OCH2); 6.43 ppm (CH).

후처리

  1. temperaturemaintaining the temperature below 10° C
  2. washwas washed three times with 1 normal hydrochloric acid
  3. dry with materialThe organic solution was dried with magnesium sulfate
  4. customthe solvent was removed at reduced pressure
  5. distillationThe residue (11.6 g) was distilled in vacuo (Bp. 61°-72° C., 3×10-3 mbar)

출처 및 근거

ORD 기록
ord-7dc503b0cd6e4260bacfbeb5224413e5
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05559266

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