Hydrochloric Acid → 3-methyl-4-[2-[N-isobutyl-N-(5-methyl-2-furylsulfonyl)amino]-4,5-dimethylphenoxymethyl]benzoic Acid

HRID 2057104ノート

反応式

HRID 2057104 の反応式
C[O:2][C:3](=[O:35])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][O:11][C:12]2[CH:17]=[C:16]([CH3:18])[C:15]([CH3:19])=[CH:14][C:13]=2[N:20]([CH2:30][CH:31]([CH3:33])[CH3:32])[S:21]([C:24]2[O:25][C:26]([CH3:29])=[CH:27][CH:28]=2)(=[O:23])=[O:22])=[C:6]([CH3:34])[CH:5]=1.Cl.C(OCC)(=O)C.O>O1CCOCC1.[OH-].[Na+].CO>[CH3:34][C:6]1[CH:5]=[C:4]([CH:9]=[CH:8][C:7]=1[CH2:10][O:11][C:12]1[CH:17]=[C:16]([CH3:18])[C:15]([CH3:19])=[CH:14][C:13]=1[N:20]([CH2:30][CH:31]([CH3:33])[CH3:32])[S:21]([C:24]1[O:25][C:26]([CH3:29])=[CH:27][CH:28]=1)(=[O:23])=[O:22])[C:3]([OH:35])=[O:2]

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 22728543Water ethylacetateHCID 588918933-methyl-4-[2-[N-isobutyl-N-(5-methyl-2-furylsulfonyl)amino]-4,5-dimethylphenoxymethyl]benzoic Acid Methyl Ester

生成物 1

HCID 102998023-methyl-4-[2-[N-isobutyl-N-(5-methyl-2-furylsulfonyl)amino]-4,5-dimethylphenoxymethyl]benzoic Acid収率 91.4%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 14798Sodium Hydroxide溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 3-methyl-4-[2-[N-isobutyl-N-(5-methyl-2-furylsulfonyl)amino]4,5-dimethylphenoxymethyl]benzoic acid methyl ester prepared in example 1 (850 mg) in dioxane (10 ml), 2N aqueous sodium hydroxide (2.5 ml) and methanol (4 ml) were added, and the mixture was stirred for 30 hours at room temperature. To the mixture, 2N hydrochloric acid was added, then ethyl acetate-water (30 ml-15 ml) was also added. The organic layer was washed, dried and concentrated under reduced pressure. The residue was dissolved in hot ethanol (40 ml) and added by hot water (40 ml), then allowed to cool. Precipitation was filtrated, and dried to give the title compound (755 mg) having the following physical data.

後処理

  1. washThe organic layer was washed
  2. customdried
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe residue was dissolved in hot ethanol (40 ml)
  5. additionadded by hot water (40 ml)
  6. temperatureto cool
  7. customPrecipitation
  8. filtrationwas filtrated
  9. customdried

出典と根拠

ORDレコード
ord-a60a74c5b5c34111b11ccad74a4f337b
出典データセット
uspto-grants-2008_02
特許番号
US07335776B2

反応ノート

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