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Hexamethylenetetramine → 2-Amino-1-cyclohexylethan-1-one hydrochloride

HRID 1062560
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HRID 1062560 반응식
Br[CH2:2][C:3]([CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1)=[O:4].C1N2CN3CN(C2)C[N:12]1C3.C(Cl)(Cl)[Cl:22]>>[ClH:22].[NH2:12][CH2:2][C:3]([CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1)=[O:4]
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참가 물질

4

반응물 3

HCID 4101HexamethylenetetramineHCID 6212ChloroformHCID 111600272-Bromo-1-cyclohexylethanone

생성물 1

HCID 222816062-Amino-1-cyclohexylethan-1-one hydrochloride수율 80%

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온도
48 °C

실험 절차

According to M6, 2.7 g (13.2 mmol) of 2-bromo-1-cyclohexylethanone (Tetrahedron, 48, 1, 67-78, 1992) are mixed with 1.92 g (13.7 mmol) of hexamethylenetetramine in 20 ml of chloroform. The mixture is heated at 48° C. for 4 hours and then evaporated to dryness. The residue is taken up in 20 ml of ethanol and 9 ml of 36% hydrochloric acid. After leaving overnight at room temperature, the reaction medium is filtered. The filtrate is evaporated to dryness to give an oil which is crystallized from diethyl ether. After filtration and drying, 2.08 g (80%) of 2-amino-1-cyclohexylethanone hydrochloride are obtained in the form of a paste.

후처리

  1. customevaporated to dryness
  2. customAfter leaving overnight at room temperature
  3. filtrationthe reaction medium is filtered
  4. customThe filtrate is evaporated to dryness
  5. customto give an oil which
  6. customis crystallized from diethyl ether
  7. filtrationAfter filtration
  8. customdrying

출처 및 근거

ORD 기록
ord-162f31b3562f4d37b14b49b48a07245d
출처 데이터셋
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06962912B2

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