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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Formic Acid → HCID 19784640, 화합물

HRID 257154
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HRID 257154 반응식
[CH:1]1([CH2:7][CH:8]2[CH:13]([OH:14])[CH2:12][C:11]([CH3:16])([CH3:15])[NH:10][C:9]2([CH3:18])[CH3:17])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH:19](O)=O.C=O.[OH-].[Na+]>O1CCOCC1>[CH:1]1([CH2:7][CH:8]2[CH:13]([OH:14])[CH2:12][C:11]([CH3:16])([CH3:15])[N:10]([CH3:19])[C:9]2([CH3:18])[CH3:17])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 284Formic AcidHCID 712FormaldehydeHCID 14798Sodium HydroxideHCID 19784639HCID 19784639, 화합물

생성물 1

HCID 19784640HCID 19784640, 화합물수율 98.5%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

반응 조건

온도
80 °C

실험 절차

Into a 100 ml-flask equipped with a thermometer, a cooling tube, a dropping funnel and a magnetic stirrer were introduced 3.8 g (15 mmol) of 3-cyclohexylmethyl-2,2,6,6-tetramethyl-4-piperidinol prepared in Example B1, 70 ml of dioxane and 0.78 g (17 mmol) of formic acid, and the content of the flask was heated to 80° C. When the temperature of the content of the flask was constant, 2.44 g (30 mmol) of 37% aqueous formaldehyde dissolved in 20 ml of dioxane was added gradually through the dropping funnel, followed by heating at the temperature for 10 hours. The content of the flask was cooled to room temperature, and 5% aqueous NaOH was added so that the pH became 8, followed by extraction with 200 ml of diethylether. The extract obtained was washed with 30 ml of water 3 times, 10 g of magnesium sulfate was added and, after it was kept standing for ca. 2 hours, the solution was filtered and concentrated to give 3.95 g (yield: 98%) of the title compound as a white solid product.

후처리

  1. customInto a 100 ml-flask equipped with a thermometer, a cooling tube, a dropping funnel and a magnetic stirrer
  2. additionwas added gradually through the dropping funnel
  3. temperatureby heating at the temperature for 10 hours
  4. temperatureThe content of the flask was cooled to room temperature
  5. extractionfollowed by extraction with 200 ml of diethylether
  6. customThe extract obtained
  7. washwas washed with 30 ml of water 3 times, 10 g of magnesium sulfate
  8. additionwas added
  9. filtrationthe solution was filtered
  10. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a58843332b3b4da5b05082d89b70e4b5
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05260443

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