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

HRID 986701ノート

反応式

HRID 986701 の反応式
[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]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 6212ChloroformHCID 20157038HCID 20157038、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f01842d832ca43f384e87ba37be2f522
出典データセット
uspto-grants-1987_12
特許番号
US04714774

反応ノート

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