Hydrochloric Acid → 4-[3-(3-Acetoxy-4-acetyl-2-propylphenoxy)propoxy]-3-bromobenzoic acid

HRID 986701노트

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HRID 986701 반응식
[C:1]([O:4][C:5]1[C:6]([CH2:35][CH2:36][CH3:37])=[C:7]([CH:29]=[CH:30][C:31]=1[C:32](=[O:34])[CH3:33])[O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:27]=[CH:26][C:16]([C:17]([O:19]C2CCCCO2)=[O:18])=[CH:15][C:14]=1[Br:28])(=[O:3])[CH3:2].Cl.C(Cl)(Cl)Cl>O1CCCC1>[C:1]([O:4][C:5]1[C:6]([CH2:35][CH2:36][CH3:37])=[C:7]([CH:29]=[CH:30][C:31]=1[C:32](=[O:34])[CH3:33])[O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:27]=[CH:26][C:16]([C:17]([OH:19])=[O:18])=[CH:15][C:14]=1[Br:28])(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6212ChloroformHCID 20157038HCID 20157038, 화합물

생성물 1

HCID 137456304-[3-(3-Acetoxy-4-acetyl-2-propylphenoxy)propoxy]-3-bromobenzoic acid수율 63%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In tetrahydrofuran (10 ml) was dissolved tetrahydropyranyl 4-[3-(3-acetoxy-4-acetyl-2-propylphenoxy)propoxy]-3-bromobenzoate (1.3 g). To the solution was added 1N HCl (1 ml), which was left standing at room temperature for one hour, followed by addition of chloroform (60 ml). The mixture was washed with water sufficiently and dried with sodium sulfate. Then, the solvent was evaporated off. The residue was crystallized with isopropyl ether, followed by recrystallization from aqueous alcohol to give 0.7 g of 4-[3-(3-acetoxy-4-acetyl-2-propylphenoxy)propoxy]-3-bromobenzoic acid as crystals, m.p. 155°-156° C.

후처리

  1. waitwas left
  2. washThe mixture was washed with water sufficiently
  3. dry with materialdried with sodium sulfate
  4. customThen, the solvent was evaporated off
  5. customThe residue was crystallized with isopropyl ether
  6. customfollowed by recrystallization from aqueous alcohol

출처 및 근거

ORD 기록
ord-f01842d832ca43f384e87ba37be2f522
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04714774

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