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Tin tetrachloride → Stannous chloride dihydrate

HRID 636364
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HRID 636364 반응식
Cl.[Cl:2][C:3]1[C:10]([Cl:11])=[CH:9][CH:8]=[C:7]([N+:12]([O-])=[O:13])[C:4]=1[CH2:5][NH2:6].[Sn:15](Cl)(Cl)([Cl:17])[Cl:16]>Cl>[OH2:13].[OH2:13].[Sn:15]([Cl:17])[Cl:16].[NH2:12][C:7]1[CH:8]=[CH:9][C:10]([Cl:11])=[C:3]([Cl:2])[C:4]=1[CH2:5][NH2:6]
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참가 물질

5

반응물 2

HCID 24287Tin tetrachlorideHCID 21255093(2,3-Dichloro-6-nitrophenyl)methanamine hydrochloride

생성물 2

HCID 61436Stannous chloride dihydrateHCID 52003502-(Aminomethyl)-3,4-dichloroaniline

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매2회

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온도
42.5 °C

실험 절차

A solution of 7.131 g of tin (II) chloride dihydrate in 4.7 L of concentrated hydrochloric acid was prepared. Separately, 1.631 g of 2,3-dichloro-6-nitrobenzylamine hydrochloride was dissolved in 9.5 L of concentrated hydrochloric acid. The solution of the amine was added to the tin chloride solution over 1-2 hours to maintain the reaction temperature below 45° C. The mixture was stirred for 2 hours at 40-45° C. in a warm water bath, and cooled in an ice/methanol bath to −5° C. The mixture was filtered, and the isolated solids slurried with 13 L water, 6.5 kg ice, and 6 L methylene chloride. Sodium hydroxide (50% aqueous solution) was added until pH >12, and the organic layer was removed. The aqueous phase was extracted with methylene chloride (2×6 L), and the combined organic layers washed with water (6 L portions) until pH=7-8. The organic layers were dried over magnesium sulfate (500 g) and charcoal (200 g) for 16 hours, and filtered. The filtrate was concentrated to an oil, and crystallized from isopropanol at −20° C. to give 2-amino-5,6-dichlorobenzylamine in 58 to 96% yield.

후처리

  1. temperatureto maintain the reaction temperature below 45° C
  2. temperaturecooled in an ice/methanol bath to −5° C
  3. filtrationThe mixture was filtered
  4. additionSodium hydroxide (50% aqueous solution) was added until pH >12
  5. customthe organic layer was removed
  6. extractionThe aqueous phase was extracted with methylene chloride (2×6 L)
  7. washthe combined organic layers washed with water (6 L portions) until pH=7-8
  8. dry with materialThe organic layers were dried over magnesium sulfate (500 g) and charcoal (200 g) for 16 hours
  9. filtrationfiltered
  10. concentrationThe filtrate was concentrated to an oil
  11. customcrystallized from isopropanol at −20° C.

출처 및 근거

ORD 기록
ord-71fb8237d79f47c49bcdf0a4ccb2b509
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06194420B1

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