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HCID 53436965, 화합물 → HCID 54162915, 화합물

HRID 704449
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HRID 704449 반응식
[C:1]([C:3]([C:7]([O:9][CH3:10])=[O:8])=[CH:4]OC)#[N:2].[N:11]1([CH:16]=[CH:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH2:15][CH2:14][CH2:13][CH2:12]1>O1CCCC1>[C:1]([C:3]([C:7]([O:9][CH3:10])=[O:8])=[CH:4][C:17]1[CH2:18][CH2:19][CH2:20][CH2:21][C:16]=1[N:11]1[CH2:15][CH2:14][CH2:13][CH2:12]1)#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 53436965HCID 53436965, 화합물HCID 538895841-(Hex-1-EN-1-YL)pyrrolidine

생성물 1

HCID 54162915HCID 54162915, 화합물수율 60.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

1-Cyano-2methoxy-1-methoxycarbonyl-ethene (8.5 g, 0.06 mol) in tetrahydrofuran (60 ml) was chilled to -25° C. At this temperature, a solution of 1-pyrrolidino-hexene (9.1 g, 0.06 mol) in tetrahydrofuran (30 ml) was added dropwise. Cooling was then stopped and the reaction mixture was allowed to warm up to room temperature. The solution was then stirred for 1 hour and then evaporated. The resulting gum was triturated with isopropanol and the resulting solid material collected by vacuum filtration. After drying, yellowish crystals of 1-cyano-1-methoxycarbonyl-2-(2-pyrrolidino-cyclohexenyl)-ethene (9.5 g, 60.9% of theoretical yield; m.pt. 133° C.-134° C.) Were obtained. The compound migrated in tlc uniformly and was used for the next step without further purification.

후처리

  1. temperatureCooling
  2. customevaporated
  3. customThe resulting gum was triturated with isopropanol
  4. filtrationthe resulting solid material collected by vacuum filtration
  5. customAfter drying

출처 및 근거

ORD 기록
ord-85e594fe76cf457e86899314bde16c14
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04987232

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