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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium Hydroxide → HCID 14854590, 화합물

HRID 974433
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HRID 974433 반응식
[C:1]([C:3]1([CH:9]([C:15]([O:17]CC)=[O:16])[C:10]([O:12]CC)=[O:11])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)#[N:2].[OH-].[Na+]>CO.O>[C:1]([C:3]1([CH:9]([C:15]([OH:17])=[O:16])[C:10]([OH:12])=[O:11])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)#[N:2]
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참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 10912488Diethyl (1-cyanocyclohexyl)propanedioate

생성물 1

HCID 14854590HCID 14854590, 화합물수율 89.9%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

50 g Diethyl (1-cyanocyclohexyl)-malonate are dissolved in 175 mL methanol at 40° C. At this temperature, a solution of 29.9 g sodium hydroxide in 150 mL water is added dropwise. The reaction mixture is stirred for 30 minutes at 40° C. After cooling to 20° C., the precipitated product (sodium salt) is filtered off with suction, the filter cake is washed with 50 mL methanol and the product is dried at 60° C. to constant weight. The product is dissolved in 500 mL of water at 10° C., and adjusted to a pH of one to two at 10-15° C. with concentrated hydrochloric acid. The substance which precipitates out is extracted three times with, in each case, 300 mL ethyl acetate. The combined ethyl acetate phases are dried and evaporated on a rotary evaporator at 35° C. The white residue obtained is dried to constant weight at 35° C. in a vacuum drying cabinet. 35.5 g of the title compound are obtained (89.8% of theory); m.p. 99.9° C.

후처리

  1. temperatureAfter cooling to 20° C.
  2. filtrationthe precipitated product (sodium salt) is filtered off with suction
  3. washthe filter cake is washed with 50 mL methanol
  4. customthe product is dried at 60° C. to constant weight
  5. dissolutionThe product is dissolved in 500 mL of water at 10° C.
  6. customadjusted to a pH of one to two at 10-15° C. with concentrated hydrochloric acid
  7. customThe substance which precipitates out
  8. extractionis extracted three times with, in each case, 300 mL ethyl acetate
  9. dry with materialThe combined ethyl acetate phases are dried
  10. customevaporated on a rotary evaporator at 35° C
  11. customThe white residue obtained
  12. customis dried to constant weight at 35° C. in a vacuum
  13. customdrying cabinet

출처 및 근거

ORD 기록
ord-49c6a01cb7a24496bd2d6b58b4f12391
출처 데이터셋
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05068413

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