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4-Chloronaphthylamine → (2-(4-(((4-Chloronaphthyl)amino)methyl)phenoxy)ethyl)diethylamine

HRID 1296850
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HRID 1296850 반응식
[CH2:1]([N:3]([CH2:15][CH3:16])[CH2:4][CH2:5][O:6][C:7]1[CH:14]=[CH:13][C:10]([CH:11]=O)=[CH:9][CH:8]=1)[CH3:2].[NH2:17][C:18]1[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[C:21]([Cl:28])=[CH:20][CH:19]=1.[BH4-].[Na+]>O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C1(C)C=CC=CC=1.CO>[Cl:28][C:21]1[C:22]2[C:27](=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:18]([NH:17][CH2:11][C:10]2[CH:13]=[CH:14][C:7]([O:6][CH2:5][CH2:4][N:3]([CH2:15][CH3:16])[CH2:1][CH3:2])=[CH:8][CH:9]=2)=[CH:19][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 784084-ChloronaphthylamineHCID 4116744-(2-(Diethylamino)-Ethoxy)-BenzaldehydeHCID 4311764Sodium borohydride

생성물 1

HCID 23514381(2-(4-(((4-Chloronaphthyl)amino)methyl)phenoxy)ethyl)diethylamine수율 2,089.2%

시약·촉매·용매 3

HCID 521998p-Toluenesulfonic acid monohydrate촉매
HCID 887
Methanol
용매
HCID 1140Toluene용매

실험 절차

A stirred solution of 0.2 gram (0.0001 mole) of 4-(2-(diethylamino)ethoxy)benzaldehyde (prepared in the manner of Step A, Example 3), 0.22 gram (0.0001 mole) of 1-amino-4-chloronaphthalene (available from Aldrich Chemical Company), and one drop of p-toluenesulfonic acid monohydrate (available from Aldrich Chemical Company) in 5 mL of toluene was heated at reflux for ten hours. At the conclusion of this period, the reaction mixture was concentrated under reduced pressure, yielding a residue. The residue was taken up in 5 mL of methanol and about 0.2 grams (0.004 mole) of sodium borohydride was added. The resulting mixture was stirred at ambient temperature for about 18 hours. After this time, the mixture was quenched with water and extracted with several portions of diethyl ether. The extracts were combined, dried with sodium sulfate and filtered. The filtrate was concentrated under reduced pressure, yielding 0.8 gram of Compound 84. The NMR spectrum was consistent with the proposed structure.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for ten hours
  3. concentrationAt the conclusion of this period, the reaction mixture was concentrated under reduced pressure
  4. customyielding a residue
  5. customAfter this time, the mixture was quenched with water
  6. extractionextracted with several portions of diethyl ether
  7. dry with materialdried with sodium sulfate
  8. filtrationfiltered
  9. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-75cb64f9bedf4ead93f4feb3873e1e84
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07247756B2

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