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Sulfuric Acid → Cyclafuramid

HRID 597257
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HRID 597257 반응식
[C:1]([O:4][CH:5]([CH3:8])[CH:6]=O)(=O)[CH3:2].[CH:9]1([NH:15][C:16](=[O:21])[CH2:17]C(C)=O)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.OS(O)(=O)=O>C1(C)C=CC=CC=1>[CH:9]1([NH:15][C:16]([C:17]2[CH:6]=[C:5]([CH3:8])[O:4][C:1]=2[CH3:2])=[O:21])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 70805N-CyclohexylacetoacetamideHCID 907282-(Acetyloxy)propanal

생성물 1

HCID 93178Cyclafuramid

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

24 parts (by weight) of α-acetoxypropionaldehyde is stirred with 36.6 parts of acetoacetic cyclohexylamide and 1 part of concentrated H2SO4 in 100 parts of toluene for 3 hours at 50° C. After the mixture has been cooled to room temperature it is washed with sodium hydrogen carbonate. The organic phase is dried with Na2SO4 and concentrated to dryness. There is obtained 41 parts of 2,5-dimethylfuran-3-carboxylic cyclohexylamide having a melting point of 111° to 113° C. After recrystallization from cyclohexane the compound melts at 114° to 115° C.

후처리

  1. washis washed with sodium hydrogen carbonate
  2. dry with materialThe organic phase is dried with Na2SO4
  3. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-14610cf6caa1447a8c7e66842238ed42
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04013684

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