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Hydrochloric Acid → HCID 20199179, 화합물

HRID 652088
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HRID 652088 반응식
O1CC[O:3][CH:2]1[C:6]1[CH:7]=[C:8]([CH:14]=[CH:15][CH:16]=1)[O:9][CH2:10][CH2:11][CH2:12][NH2:13].CS[C:19]([N:33]([CH3:42])[N:34]=CC1C=CC=CC=1)=[N:20][C:21](=O)[CH2:22][S:23]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)(=[O:25])=[O:24].Cl.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1.CC(C)=O>[CH3:42][N:33]1[C:19]([NH:13][CH2:12][CH2:11][CH2:10][O:9][C:8]2[CH:7]=[C:6]([CH:16]=[CH:15][CH:14]=2)[CH:2]=[O:3])=[N:20][C:21]([CH2:22][S:23]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)(=[O:25])=[O:24])=[N:34]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 127974473-[3-(1,3-Dioxolan-2-yl)phenoxy]propanamineHCID 54365749methyl-1-methyl-2-(phenylmethylene)-N-[2-(phenylsulphonyl)acetyl]hydrazine carboximidothioate

생성물 1

HCID 20199179HCID 20199179, 화합물수율 70.5%

시약·촉매·용매 2

HCID 180
Acetone
용매
HCID 1140Toluene용매

실험 절차

A mixture of 3-[3-(1,3-dioxolan-2-yl)phenoxy]propanamine (2.3 g) and methyl-1-methyl-2-(phenylmethylene)-N-[2-(phenylsulphonyl)acetyl]hydrazine carboximidothioate (4.0 g) was heated at 60° under water pump vacuum for 3 h. The reaction mixture was dissolved in toluene (100 ml), 5N hydrochloric acid (100 ml) and acetone (50 ml) and stirred at room temperature for 18 h. The aqueous layer was basified to pH 9 with potassium carbonate and extracted with ethyl acetate. The organic extract was evaporated to give the title compound as an amber gum (3.0 g) T.l.c. Methanol; Rf 0.8.

후처리

  1. temperaturewas heated at 60° under water
  2. customfor 3 h
  3. extractionextracted with ethyl acetate
  4. extractionThe organic extract
  5. customwas evaporated

출처 및 근거

ORD 기록
ord-636c917019a2411982d19ecbd6fe0505
출처 데이터셋
uspto-grants-1987_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04670448

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