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Acetic Acid → 3-(2,3-dihydro-1,4-benzodioxin-2-yl)propanoic acid

HRID 1388680
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반응식

HRID 1388680 반응식
C(C[CH2:4][CH:5]1[O:10][C:9]2[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=2[O:7][CH2:6]1)#N.S(=O)(=O)(O)O.[C:20]([OH:23])(=[O:22])[CH3:21]>O>[O:10]1[C:9]2[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=2[O:7][CH2:6][CH:5]1[CH2:4][CH2:21][C:20]([OH:23])=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 12761751HCID 12761751, 화합물

생성물 1

HCID 2675483-(2,3-dihydro-1,4-benzodioxin-2-yl)propanoic acid

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

72 g 2-(2-cyanoethyl) (2,3-dihydro [4H] 1,4-benzodioxin) are suspended in 100 ml acetic acid, 100 ml water and 40 g sulphuric acid. The whole is heated to reflux for 48 hours and the mixture is thereafter poured in water. The aqueous phase is extracted with ether. The ethereous solution is separated, washed, dried and concentrated off. 76 g of 3-(2,3-dihydro [4H] 1,4-benzodioxin-2 yl) propionic acid are obtained, melting at 102°. This acid is esterified with methanol and p toluene sulphonic acid at the boiling point for 18 hours. After the usual purifications 71 g of the methyl ester are obtained. MP: 55°.

후처리

  1. temperatureThe whole is heated
  2. temperatureto reflux for 48 hours
  3. extractionThe aqueous phase is extracted with ether
  4. customThe ethereous solution is separated
  5. washwashed
  6. customdried
  7. concentrationconcentrated off

출처 및 근거

ORD 기록
ord-9264f73597eb41c196594f99a2ed0e9d
출처 데이터셋
uspto-grants-1984_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04432984

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