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Hydrochloric Acid → HCID 178481944, 화합물

HRID 1089040
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HRID 1089040 반응식
[CH3:1][NH:2][C:3]([C:10]([F:13])([F:12])[F:11])=[CH:4][C:5](OCC)=[O:6].C[NH:15]N.Cl>O>[CH3:1][N:2]1[C:3]([C:10]([F:13])([F:12])[F:11])=[CH:4][C:5]([OH:6])=[N:15]1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6061MethylhydrazineHCID 27588682-Butenoic acid, 4,4,4-trifluoro-3-(methylamino)-, ethyl ester

생성물 1

HCID 178481944HCID 178481944, 화합물수율 42.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A 50 ml. flask equipped with mechanical stirrer and reflux condenser was charged with 19.7 g of ethyl 3-methylamino-4,4,4-trifluoro-2-butenoate and 4.8 g of methylhydrazine and heated to 50°-65° C. for 2.75 hr., then to 40°-45° C. for 2 hr., and then allowed to cool to room temperature and stand overnight. The clear reaction mixture was taken up in 15 ml. of water and conc. hydrochloric acid added dropwise to pH 6.0-6.5 which required 5.2 ml. of acid. The precipitated product was collected by filtration and dried to obtain 7.06 g (42.5%) of product m.p. 127°-128.5° C.

후처리

  1. customflask equipped with mechanical stirrer
  2. temperaturereflux condenser
  3. temperatureheated to 50°-65° C. for 2.75 hr
  4. waitstand overnight
  5. filtrationThe precipitated product was collected by filtration
  6. customdried

출처 및 근거

ORD 기록
ord-d5adaaa05297444daaf31e3fd61804e0
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04964895

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