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Hydrochloric Acid → 3-Phenylbutyl acetate

HRID 1938107
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HRID 1938107 반응식
[C:1]1([CH:7]([CH3:11])[CH2:8][CH2:9][OH:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1(C)C=CC=CC=1.[C:19](OC(=O)C)(=[O:21])[CH3:20].Cl>CN(C)C1C=CN=CC=1.N1C=CC=CC=1>[C:19]([O:10][CH2:9][CH2:8][CH:7]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[CH3:11])(=[O:21])[CH3:20]
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 1140TolueneHCID 7918Acetic AnhydrideHCID 94243Benzenepropanol, gamma-methyl-

생성물 1

HCID 30164553-Phenylbutyl acetate수율 99%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매
HCID 1049
Pyridine
용매

실험 절차

Into a four-necked flask provided with a stirring means and a thermometer, 150 g (1 mol) of (+)-3-phenyl-1-butanol (XXVI-60), 500 ml of toluene and 200 ml of pyridine were charged, and 122.4 g (1.2 mol) of acetic acid anhydride and 1 g of 4-dimethylaminopyridine were further added thereto. The mixture was reacted for 4 hours while temperature being maintained at 40°-50° C. After completion of the reaction, the reaction mixture was poured into 500 ml of 4N hydrochloric acid, extracted and fractionated. The resulting organic layer was washed with 1N hydrochloric acid, water, 5% sodium bicarbonate aqueous solution ad water in the order. The thus-obtained organic layer was concentrated under a reduced pressure to obtain 190 g of (+)-1-acetoxy-3-phenylbutane (XXV-60) with yield of 99.0%.

후처리

  1. customInto a four-necked flask provided with a stirring means
  2. customThe mixture was reacted for 4 hours while temperature
  3. temperaturebeing maintained at 40°-50° C
  4. customAfter completion of the reaction
  5. extractionextracted
  6. washThe resulting organic layer was washed with 1N hydrochloric acid, water, 5% sodium bicarbonate aqueous solution ad water in the order
  7. concentrationThe thus-obtained organic layer was concentrated under a reduced pressure

출처 및 근거

ORD 기록
ord-1e8c16cae6b446ad8147a8e06dbad788
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05693251

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