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Triethylamine → 4-(3,4-Dihydro-1H-benzo[4,5]thieno[2,3-c]pyridine-2-sulfonylmethyl)-tetrahydro-pyran-4-carboxylic acid

HRID 992435
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HRID 992435 반응식
C[O:2][C:3]([C:5]1([CH2:11][S:12](Cl)(=[O:14])=[O:13])[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1)=[O:4].Cl.[CH2:17]1[C:22]2[S:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[C:21]=2[CH2:20][CH2:19][NH:18]1.C(N(CC)CC)C.O.[OH-].[Li+]>O1CCCC1.CO.O>[CH2:17]1[C:22]2[S:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[C:21]=2[CH2:20][CH2:19][N:18]1[S:12]([CH2:11][C:5]1([C:3]([OH:2])=[O:4])[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1)(=[O:14])=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 168937Lithium hydroxide, monohydrateHCID 122652651,2,3,4-Tetrahydro-[1]benzothieno[2,3-c]pyridine hydrochlorideHCID 22228396Methyl 4-[(chlorosulfonyl)methyl]oxane-4-carboxylate

생성물 1

HCID 102007324-(3,4-Dihydro-1H-benzo[4,5]thieno[2,3-c]pyridine-2-sulfonylmethyl)-tetrahydro-pyran-4-carboxylic acid수율 25.4%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

4-Chlorosulfonylmethyl-tetrahydro-pyran-4-carboxylic acid methyl ester (520 mg) was added to a solution of 1,2,3,4-tetrahydrobenzo[4,5]thieno[2,3-c]pyridine hydrochloride (450 mg) and triethlyamine (1.0 ml) in tetrahydrofuran (20 ml). The mixture was stirred at room temperature for 18 h then water (5 ml), methanol (5 ml) and lithium hydroxide monohydrate (400 mg) were added and the reaction heated to reflux for 3 h. The mixture was evaporated under reduced pressure and the aqueous residue washed with diethyl ether (2×10 ml), acidified with 1M hydrochloric acid and the precipitate collected by filtration to give the title compound (200 mg, 25%) as a white solid.

후처리

  1. temperaturethe reaction heated
  2. temperatureto reflux for 3 h
  3. customThe mixture was evaporated under reduced pressure
  4. washthe aqueous residue washed with diethyl ether (2×10 ml)
  5. filtrationthe precipitate collected by filtration

출처 및 근거

ORD 기록
ord-b0238baf35594c81a7b0b0a173b75af6
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06469020B2

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