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Hydrochloric Acid → HCID 67598367, 화합물

HRID 1417305
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HRID 1417305 반응식
C([NH:9][CH2:10][C:11]1[S:15][C:14]([S:16](Cl)(=[O:18])=[O:17])=[CH:13][CH:12]=1)(=O)C1C=CC=CC=1.Cl.Cl.[N:22]1([C:27]2[CH:38]=[CH:37][C:30]([O:31][CH2:32][CH2:33][CH2:34][CH2:35][NH2:36])=[CH:29][CH:28]=2)[CH:26]=[CH:25][N:24]=[CH:23]1.[OH-].[Na+].Cl>ClCCl.O>[NH2:9][CH2:10][C:11]1[S:15][C:14]([S:16]([NH:36][CH2:35][CH2:34][CH2:33][CH2:32][O:31][C:30]2[CH:37]=[CH:38][C:27]([N:22]3[CH:26]=[CH:25][N:24]=[CH:23]3)=[CH:28][CH:29]=2)(=[O:17])=[O:18])=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 27788785-(Benzamidomethyl)thiophene-2-sulfonyl chlorideHCID 67693419HCID 67693419, 화합물

생성물 1

HCID 67598367HCID 67598367, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 6344
Dichloromethane
용매

실험 절차

A solution of 3.0 g of 5-benzoylaminomethyl-2-thiophenesulfonyl chloride, in 100 ml of dichloromethane, is added to a stirred mixture of 3.0 g of 4-[4-(1H-imidazol-1-yl)phenoxy]butaneamine dihydrochloride (Example 2) and 3.5 ml of 10N NaOH in 100 ml of water. The mixture is stirred at room temperature for 3 hours, a tacky precipitate being formed. The precipitate is mixed with 100 ml of concentrate HCl, and the mixture is stirred at reflux for 12 hours, solution taking place. The solution is taken to dryness in vacuo, and the dihydrochloride salt of the title compound was recrystallized from aqueous ethanol, m.p. 230°-232° C. (dec.); yield, 0.5 g.

후처리

  1. customa tacky precipitate being formed
  2. stirringthe mixture is stirred
  3. temperatureat reflux for 12 hours
  4. customthe dihydrochloride salt of the title compound was recrystallized from aqueous ethanol, m.p. 230°-232° C. (dec.)
  5. customyield

출처 및 근거

ORD 기록
ord-c7138074a7af4c43ab2385214e399304
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05877196

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