Formaldehyde → HCID 178481284, 화합물

HRID 1290997노트

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HRID 1290997 반응식
[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([OH:8])[CH2:4][CH2:3]1.[CH3:9][N:10](C)[C:11](N)=O.C=[O:16].[CH3:17][N:18]1[CH2:23]COC[CH2:19]1>C1(C)C=CC=CC=1.O1CCOCC1>[OH:8][C@H:5]1[CH2:6][CH2:7][C@H:2]([N:1]2[CH2:9][N:10]([CH3:11])[C:23](=[O:16])[N:18]([CH3:17])[CH2:19]2)[CH2:3][CH2:4]1

참가 물질

7

반응물 4

HCID 712FormaldehydeHCID 79724-MethylmorpholineHCID 11737N,N-DimethylureaHCID 178511715HCID 178511715, 화합물

생성물 1

HCID 178481284HCID 178481284, 화합물수율 75%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 312751,4-Dioxane용매

실험 절차

To a mixture of trans-4-aminocyclohexanol (5.00 g, 43.4 mmol), N,N-dimethylurea (3.82 g, 43.4 mmol), 37% formalin (50 ml), N-methylmorpholine (9.54 ml, 86.8 mmol) and dioxane (10 ml) was added toluene (200 ml), and the mixture was heated for about 5 hours while removing water for azeotropic distillation. Low boiling matters were distilled away from the reaction mixture under reduced pressure, and the residue was purified by silica gel column chromatography (methylene chloride/methanol=50/1-10/1) to give 7.40 g of trans-5-(4-hydroxycyclohexyl)-1,3-dimethylhexahydro-2-oxo-1,3,5-triazine as colorless solid (75%).

후처리

  1. temperaturethe mixture was heated for about 5 hours
  2. customwhile removing water
  3. distillationfor azeotropic distillation
  4. distillationwere distilled away from the reaction mixture under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (methylene chloride/methanol=50/1-10/1)

출처 및 근거

ORD 기록
ord-6c42842c47cc4db78bd37a9ead13f8bc
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753670

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