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Hydrochloric Acid → HCID 1490650, 화합물

HRID 616396
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HRID 616396 반응식
[C:1]1(=[O:10])[O:9][C:6]([CH3:8])([CH3:7])[O:5][C:3](=[O:4])[CH2:2]1.C(N(CC)CC)C.[Cl:18][C:19]1[CH:20]=[C:21]([N:26]=[C:27]=[O:28])[CH:22]=[CH:23][C:24]=1[Cl:25].Cl>CS(C)=O.O>[CH3:7][C:6]1([CH3:8])[O:9][C:1](=[O:10])[C:2]([C:27](=[O:28])[NH:26][C:21]2[CH:22]=[CH:23][C:24]([Cl:25])=[C:19]([Cl:18])[CH:20]=2)=[C:3]([OH:4])[O:5]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 76073,4-Dichlorophenyl isocyanateHCID 8471TriethylamineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dione

생성물 1

HCID 1490650HCID 1490650, 화합물

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매2회
HCID 962
Water
용매

실험 절차

To a solution of 14.4 g of isopropylidene malonate in 150 ml of dimethyl sulphoxide were added dropwise, at room temperature, 10.1 g of triethylamine and thereafter, at 20° to 30° C, 18.8 g of 3,4-dichlorophenylisocyanate in 30 ml of dimethyl sulphoxide. The mixture was reacted for 12 to 15 hours at room temperature and the resultant solution was poured into a solution of 20 ml of concentrated hydrochloric acid in 200 ml of water. The precipitate which formed was collected with suction. Recrystallisation from 130 ml of acetone yielded the product of the formula ##STR5## with a melting point of 132°-134° C.

후처리

  1. customat 20° to 30° C
  2. customThe mixture was reacted for 12 to 15 hours at room temperature
  3. customThe precipitate which formed
  4. customwas collected with suction
  5. customRecrystallisation from 130 ml of acetone
  6. customyielded the product of the formula ##STR5## with a melting point of 132°-134° C.

출처 및 근거

ORD 기록
ord-182466c2282648d3a5461bcd894e5c10
출처 데이터셋
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04073932

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