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Sulfamic Acid → HCID 11447496, 화합물

HRID 582761
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HRID 582761 반응식
[S:1](=[O:5])(=[O:4])([OH:3])N.[C:6]1([NH2:16])[C:15]2[CH2:14][CH2:13][CH2:12][CH2:11][C:10]=2[CH:9]=[CH:8][CH:7]=1>CN1CCCC1=O.ClC1C=CC=CC=1Cl>[NH2:16][C:6]1[C:15]2[CH2:14][CH2:13][CH2:12][CH2:11][C:10]=2[C:9]([S:1]([OH:3])(=[O:5])=[O:4])=[CH:8][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 5987Sulfamic AcidHCID 166715-Tetralinylamine

생성물 1

HCID 11447496HCID 11447496, 화합물수율 48.6%

시약·촉매·용매 2

HCID 72391,2-Dichlorobenzene용매HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
150 °C

실험 절차

A hot suspension of 20 g of sulphamic acid in 40 ml of N-methylpyrrolidone is added to a solution of 10 g of 5,6,7,8-tetrahydronaphthylamine in 100 ml of 1,2-dichlorobenzene. The mixture is heated with stirring for 7 hours at 150° C. The product is filtered off and washed with dichlorobenzene and then with toluene. The precipitate is resuspended in 70 ml of water and neutralized to pH 7 with 5.5 ml of 30% sodium hydroxide. The insoluble matter is filtered off and the aqueous phase is extracted with ether. The aqueous phase is adjusted to pH 5 by adding HCl, at 5° C.; the mixture is filtered, and the residue is washed with water and dried to obtain 7.5 g of the expected product.

후처리

  1. temperatureThe mixture is heated
  2. filtrationThe product is filtered off
  3. washwashed with dichlorobenzene
  4. filtrationThe insoluble matter is filtered off
  5. extractionthe aqueous phase is extracted with ether
  6. additionby adding HCl
  7. customat 5° C.
  8. filtrationthe mixture is filtered
  9. washthe residue is washed with water
  10. customdried

출처 및 근거

ORD 기록
ord-4abdbeb762474c8888646d4d598df885
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05925661

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