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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → p-Toluenesulfonic acid

HRID 396944
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HRID 396944 반응식
Cl.[K].NC1C=CC(F)=CC=1S.O.[C:13]1([CH3:23])[CH:18]=[CH:17][C:16]([S:19]([OH:22])(=[O:21])=[O:20])=[CH:15][CH:14]=1>O1CCCC1.O>[CH3:23][C:13]1[CH:18]=[CH:17][C:16]([S:19]([OH:22])(=[O:21])=[O:20])=[CH:15][CH:14]=1
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 3205472-Amino-5-fluorobenzene-1-thiolHCID 521998p-Toluenesulfonic acid monohydrateHCID 5462222Potassium

생성물 1

HCID 6101p-Toluenesulfonic acid수율 174.2%

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

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온도
1 °C

실험 절차

80 ml of water and 60 g (0.592 mole) of 36% hydrochloric acid were placed in a 500-ml flask as a reactor, and cooled to 0 to 2° C. Thereto was dropwise added, at 0 to 5° C. with stirring, 96.0 g (0.112 mole) of an aqueous solution of a potassium salt of 2-amino-5-fluorothiophenol. The resulting mixture had a pH of 0.90. Further, 20.0 g (0.105 mole) of p-toluenesulfonic acid monohydrate was added. Thereto was dropwise added, at 16 to 20° C., a solution of D-alanine-N-carboxyanhydride (16.7 g, purity: 78.3%, 0.318 mole) dissolved in tetrahydrofuran (30 ml) (the solution was beforehand prepared at 16 to 20° C.). Aging was conducted at 15 to 20° C. for 4 hours. The resulting crystals were collected by filtration and dried at 60° C. to obtain 31.5 g of a p-toluenesulfonate of [2-(6-fluorobenzothiazolyl)]ethylamine (purity: 98.95%) (the yield was 75.5% relative to the potassium salt of 2-amino-5-fluorothiophenol).

후처리

  1. additionThereto was dropwise added, at 0 to 5° C.
  2. additionThereto was dropwise added, at 16 to 20° C.
  3. customwas beforehand prepared at 16 to 20° C.)
  4. filtrationThe resulting crystals were collected by filtration
  5. customdried at 60° C.

출처 및 근거

ORD 기록
ord-59038b25679d41f3b1264152b43796f4
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06608207B2

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