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Formaldehyde → HCID 68109090, 화합물

HRID 385104
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HRID 385104 반응식
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[NH:3][CH2:2]1.NC1C=CC=CC=1S.C=O.[C:20]([C:24]1[CH:25]=[C:26]([CH:30]=[C:31]([S:35]([CH3:38])(=[O:37])=[O:36])[C:32]=1[O:33][CH3:34])[C:27](Cl)=[O:28])([CH3:23])([CH3:22])[CH3:21]>C(Cl)(Cl)Cl.C(N(CC)CC)C>[C:20]([C:24]1[CH:25]=[C:26]([CH:30]=[C:31]([S:35]([CH3:38])(=[O:36])=[O:37])[C:32]=1[O:33][CH3:34])[C:27]([N:3]1[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[S:1][CH2:2]1)=[O:28])([CH3:23])([CH3:21])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 712FormaldehydeHCID 87132-AminothiophenolHCID 96588BenzothiazolineHCID 86668171HCID 86668171, 화합물

생성물 1

HCID 68109090HCID 68109090, 화합물

시약·촉매·용매 2

HCID 6212Chloroform용매
HCID 8471
Triethylamine
용매

실험 절차

2,3-dihydro-1,3-benzothiazole synthesized from 2-aminobenzenethiol (182 mg) and 37% formalin (87 μL) in the same manner as in Example 1 was dissolved in chloroform (4 mL), and triethylamine (0.29 mL) and 3-t-butyl-4-methoxy-5-methanesulfonylbenzoyl chloride were added to the solution, and then the mixture was stirred at room temperature for 1 hour. The solvent was distilled off under reduced pressure, water was added and then the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1) to obtain the title compound (246 mg) as a pale yellow amorphous product.

후처리

  1. distillationThe solvent was distilled off under reduced pressure, water
  2. additionwas added
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off under reduced pressure
  7. customthe obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-4034fa81b4414e929395c1b37b7c63d6
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367843B2

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