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Water → HCID 11057721, 화합물

HRID 1244791
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HRID 1244791 반응식
FC(F)(F)C(O)=O.O.[Cl:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][CH:19]=1)[CH:16]=[C:15]([S:20]([N:23]([CH2:30][CH:31](OCC)[O:32]CC)[CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])(=[O:22])=[O:21])[CH:14]=[CH:13]2.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[Cl:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][CH:19]=1)[CH:16]=[C:15]([S:20]([N:23]([CH2:30][CH:31]=[O:32])[CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])(=[O:22])=[O:21])[CH:14]=[CH:13]2
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참가 물질

6

반응물 4

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 11812307Ethyl 2-[(6-chloronaphthalen-2-ylsulfonyl)(2,2-diethoxyethyl)amino]acetate

생성물 1

HCID 11057721HCID 11057721, 화합물수율 51.4%

시약·촉매·용매 1

HCID 6212
Chloroform
용매
2회

실험 절차

To a mixed solution of trifluoroacetic acid (5 ml), chloroform (1.5 ml) and water (2.5 ml) was added a solution of the compound obtained in Step 2 (560 mg) in chloroform (1 ml) under cooling with ice water. After stirring for 1.5 hours under cooling with ice water, the reaction mixture was adjusted to pH 8 with saturated aqueous solution of sodium hydrogencarbonate and extracted with diethyl ether. The organic layer was dried over anhydrous sodium sulfate and thereafter the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=5:1–2:1) to obtain the title compound (240 mg).

후처리

  1. extractionextracted with diethyl ether
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=5:1–2:1)

출처 및 근거

ORD 기록
ord-e6e2e3aecd36423bafbf74e6c67e2da7
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07122662B2

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