Potassium Carbonate → HCID 58579786, 화합물

HRID 1918458노트

반응식

HRID 1918458 반응식
[C:1]1([N:7]=[C:8]([S:15][CH2:16][CH:17]2[CH2:19][CH2:18]2)[C:9]#[C:10][Si](C)(C)C)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)([O-])[O-].[K+].[K+].[F:26][C:27]1[CH:32]=[CH:31][C:30]([SH:33])=[CH:29][CH:28]=1>CO>[F:26][C:27]1[CH:32]=[CH:31][C:30]([S:33][CH:10]=[CH:9][C:8](=[N:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[S:15][CH2:16][CH:17]2[CH2:19][CH2:18]2)=[CH:29][CH:28]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 677894-FluorothiophenolHCID 58579770HCID 58579770, 화합물

생성물 1

HCID 58579786HCID 58579786, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Cyclopropylmethyl N-phenyl-3-(trimethylsilyl)thiopropynimidate (0.91 g) was dissolved in methanol (15 mL), a small amount of potassium carbonate was dissolved thereto at room temperature, and the mixture was stirred for 1 hour. 4-fluorothiophenol (0.35 mL) was added thereto and further stirred for 5.5 hours. The reaction mixture was concentrated under reduced pressure, then the residue was subjected to silica gel column chromatography (hexane/ethyl acetate=20/1), medium pressure HPLC (hexane/ethyl acetate=99.2/0.8-98.5/1.5) to obtain cyclopropylmethyl 3-(4-fluorophenylthio)-N-(phenyl)thioacrylimidate (0.84 g).

후처리

  1. stirringfurther stirred for 5.5 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e5885224ca61461491a19b2712ca63df
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618329B2

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