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Hydrochloric Acid → HCID 20137673, 화합물

HRID 1252844
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HRID 1252844 반응식
[CH2:1]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15]#[N:16])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9].C([Li])CCC.[C:22](OCC)(=[O:24])[CH3:23].Cl>O1CCCC1.CCCCCC.O>[C:22]([CH:14]([CH2:13][CH2:12][CH2:11][O:10][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9])[C:15]#[N:16])(=[O:24])[CH3:23]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 20137668HCID 20137668, 화합물HCID 178418339Butyllithium

생성물 1

HCID 20137673HCID 20137673, 화합물

시약·촉매·용매 3

HCID 962Water용매2회
HCID 8028
Tetrahydrofuran
용매
2회
HCID 8058Hexane용매

반응 조건

온도
-60 °C

실험 절차

35.0 g (156 millimoles) of 5-(n-nonyloxy)-valeronitrile in 500 ml of absolute tetrahydrofuran are initially taken, in the absence of water and under an inert gas atmosphere, and the mixture is cooled to -60° C. 162 millimoles of n-butyl-lithium in n-hexane are slowly added to the stirred mixture, which is then left for 4 hours at -60° C. A solution of 13.1 g (155 millimoles) of dry ethyl acetate in tetrahydrofuran is then added dropwise, stirring is continued for 3 hours at -60° C., and the mixture is allowed to warm up slowly to room temperature. First water and then 2N hydrochloric acid are added while cooling with ice, until the pH of the solution reaches 4. The organic phase which separates out is isolated, washed with water, dried and evaporated down. The oil which remains (41 g; 99%) is more than 90% pure according to gas chromatography, and can be reacted without further purification.

후처리

  1. waitis continued for 3 hours at -60° C.
  2. temperatureto warm up slowly to room temperature
  3. temperaturewhile cooling with ice, until the pH of the solution
  4. customThe organic phase which separates out is isolated
  5. washwashed with water
  6. customdried
  7. customevaporated down
  8. customcan be reacted without further purification

출처 및 근거

ORD 기록
ord-25f57552c1bb430eb838e9416117862d
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE032676

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