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Hydrochloric Acid → 7-[4-(2-Propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid

HRID 413603
ノート
印刷プレビュー

反応式

HRID 413603 の反応式
[CH2:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[CH:15]=[CH:16][C:17]3[S:23](=[O:25])(=[O:24])[CH2:22][CH2:21][C:20]([C:26]([O:28]CC)=[O:27])=[CH:19][C:18]=3[CH:31]=2)=[CH:10][CH:9]=1)[CH2:2][CH3:3].O.C(=O)([O-])[O-].[K+].[K+].Cl>O1CCCC1.CO>[CH2:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[CH:9]=[CH:10][C:11]([C:14]2[CH:15]=[CH:16][C:17]3[S:23](=[O:24])(=[O:25])[CH2:22][CH2:21][C:20]([C:26]([OH:28])=[O:27])=[CH:19][C:18]=3[CH:31]=2)=[CH:12][CH:13]=1)[CH2:2][CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962Water2 回HCID 11430Potassium CarbonateHCID 70033921Ethyl 7-(4-propoxyethoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxlate

生成物 1

HCID 219958267-[4-(2-Propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid収率 91.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

Ethyl 7-(4-propoxyethoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxlate (11 g, 24.7447 mmol) was dissolved in 110 ml of tetrahydrofuran and 55 ml of methanol, and then 93.5 ml of water was added. After adding potassium carbonate (6.84 g, 49.49 mmol), the mixture was heated under reflux for 4.5 hours. Under reflux, 39.6 ml of a 3N hydrochloric acid and 40 ml of water were dropped. After cooling, the mixture was stirred for 1 hour while cooling in ice. After filtration, the residue was washed with 88 ml of water. After vacuum drying (40° C.), 9.4 g (Yield 91.2%) of 7-(4-propoxyethoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid was obtained as pale yellowish white crystals.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 4.5 hours
  3. temperatureUnder reflux
  4. temperatureAfter cooling
  5. temperaturewhile cooling in ice
  6. filtrationAfter filtration
  7. washthe residue was washed with 88 ml of water
  8. customAfter vacuum drying (40° C.)

出典と根拠

ORDレコード
ord-1d5c1dc62ec148eead03e25b0f4511cd
出典データセット
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06566535B1

反応ノート

読み込み中…

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