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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Methanol → HCID 19374854, 화합물

HRID 128688
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HRID 128688 반응식
[CH2:1]([NH2:4])[CH2:2][CH3:3].[CH:5]1([C:8]([CH2:10][CH:11]2[CH2:13][CH2:12]2)=O)[CH2:7][CH2:6]1.CO.[BH4-].[Na+]>C(Cl)Cl.[Ti](Cl)(Cl)(Cl)Cl.O>[CH:5]1([CH:8]([NH:4][CH2:1][CH2:2][CH3:3])[CH2:10][CH:11]2[CH2:13][CH2:12]2)[CH2:7][CH2:6]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 887MethanolHCID 7852PropylamineHCID 4311764Sodium borohydrideHCID 132271681,2-Dicyclopropylethan-1-one

생성물 1

HCID 19374854HCID 19374854, 화합물

시약·촉매·용매 3

HCID 24193Titanium Tetrachloride촉매
HCID 962
Water
용매
HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

Add 6.9 ml of propylamine to 2.2 g of cyclopropylmethyl cyclopropyl ketone in 85 ml of methylene chloride. Add 7 ml of a 1M solution of titanium (IV) chloride in methylene chloride dropwise at room temperature. After 18 hours stirring, add 40 ml of anhydrous methanol. Cool to 0° C. and add 1.0 g of sodium borohydride in small amounts. After overnight stirring at room temperature, add 10 ml of water and evaporate under vacuum. Take up in water and extract with methylene chloride. Extract with 2N hydrochloric acid. Wash with ethyl ether. Neutralise the aqueous phase with concentrated sodium hydroxide solution. Extract with methylene chloride, dry over anhydrous sodium sulphate and evaporate to dryness to obtain a colourless oil.

후처리

  1. stirringAfter overnight stirring at room temperature
  2. customevaporate under vacuum
  3. extractionextract with methylene chloride
  4. extractionExtract with 2N hydrochloric acid
  5. washWash with ethyl ether
  6. extractionExtract with methylene chloride
  7. dry with materialdry over anhydrous sodium sulphate
  8. customevaporate to dryness
  9. customto obtain a colourless oil

출처 및 근거

ORD 기록
ord-05887d6a0d3f491ab44eb622077f52b2
출처 데이터셋
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05464847

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