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Hydrochloric Acid → HCID 131721513, 화합물

HRID 612383
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HRID 612383 반응식
[Cl:1][C:2]1[CH:23]=[C:22]([Cl:24])[CH:21]=[CH:20][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([S:16](Cl)(=[O:18])=[O:17])[CH:8]=[CH:9][C:10]=1[NH:11][S:12]([CH3:15])(=[O:14])=[O:13].[NH:25]1[CH2:30]C[O:28]CC1.[OH-:31].[Na+].Cl>O1CCOCC1>[N:11]1([C:30]([NH2:25])=[O:31])[CH2:10][CH2:5][O:4][CH2:3][CH2:20]1.[Cl:1][C:2]1[CH:23]=[C:22]([Cl:24])[CH:21]=[CH:20][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([S:16]([OH:28])(=[O:18])=[O:17])[CH:8]=[CH:9][C:10]=1[NH:11][S:12]([CH3:15])(=[O:14])=[O:13]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8083MorpholineHCID 14798Sodium HydroxideHCID 23221647HCID 23221647, 화합물

생성물 1

HCID 131721513HCID 131721513, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

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온도
0 °C

실험 절차

3-(2,4-Dichlorophenoxy)-4-methylsulphonylaminobenzene-sulphonic acid chloride (1.36 g, 3.2 mmol) was dissolved in dioxan (5 ml) and at 0° C. added dropwise to a solution of morpholine (2.25 ml, 25.6 mmol) in 1N aqueous NaOH (26 ml, 26 mmol) and dioxan (20 ml). The mixture was stirred for 1 hour at 0° C., acidified with 1N HCl and extracted with ethyl acetate. The combined organic phases were dried over MgSO4 and the solvent was evaporated off. The residue was purified by chromatography (silica gel, CH2Cl2 /ethyl acetate 9/1). Yield: 0.93 g=60% 13C (100 MHz, DMSO-d6) δ 150.02, 147.15, 133.44, 130.43, 129.51, 129.31, 129.18, 126.23, .125.98, 123.95, 123.02, 122.51, 116.78, 115.83, 65.41, 45.83, 41.03

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined organic phases were dried over MgSO4
  3. customthe solvent was evaporated off
  4. customThe residue was purified by chromatography (silica gel, CH2Cl2 /ethyl acetate 9/1)

출처 및 근거

ORD 기록
ord-0a6fb0b29ab8454997dea205491da628
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06004948

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