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Hydrochloric Acid → HCID 13881294, 화합물

HRID 231579
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HRID 231579 반응식
Cl[S:2]([C:5]1[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[C:6]=1[C:7]([O:9][CH3:10])=[O:8])(=[O:4])=[O:3].[NH2:18][CH2:19][CH2:20][CH2:21][OH:22].Cl>C1COCC1>[OH:22][CH2:21][CH2:20][CH2:19][NH:18][S:2]([C:5]1[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[C:6]=1[C:7]([O:9][CH3:10])=[O:8])(=[O:4])=[O:3]
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 90863-Amino-1-propanolHCID 13670189Methyl 2-(chlorosulfonyl)-6-nitrobenzoate

생성물 1

HCID 13881294HCID 13881294, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of methyl 2-chlorosulfonyl-6-nitrobenzoate (2.80g, 10 mmol) in 100 ml of THF was cooled to ice temperature and stirred in an ice-bath while a solution of 3-amino-1-propanol (99%) (1.67g, 22 mmol) was added dropwise over a period of 45 minutes. Stirring in the ice-bath was continued for 30 minutes. The reaction miture than was acidified by addition of 3.0 ml of 1.2N HCl. The THF was evaporated under reduced pressure and the residue taken up in 100 ml of ethyl acetate. After extracting this solution with 4×20 ml of saturated NaCl solution, the ethyl acetate was evaporated and the residue recrystallized from a mixture of ethyl acetate and hexane to give 2.70g (84.9%) of light yellow crystalline product, m.p., 87-88.5°.

후처리

  1. additionwas added dropwise over a period of 45 minutes
  2. customThe THF was evaporated under reduced pressure
  3. extractionAfter extracting this solution with 4×20 ml of saturated NaCl solution
  4. customthe ethyl acetate was evaporated
  5. customthe residue recrystallized from a mixture of ethyl acetate and hexane
  6. customto give 2.70g (84.9%) of light yellow crystalline product, m.p., 87-88.5°

출처 및 근거

ORD 기록
ord-395cd1fe17174bf9804b6379f43a918a
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04847294

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