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Carbonochloridothioic acid, S-phenyl ester → (1-cyano1-methylethyl)carbamothioic acid, S-phenyl ester

HRID 65798
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HRID 65798 반응식
[NH2:1][C:2]([CH3:6])([CH3:5])[C:3]#[N:4].[C:7]1([S:13][C:14](Cl)=[O:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>O1CCOCC1>[C:3]([C:2]([NH:1][C:14](=[O:15])[S:13][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)([CH3:6])[CH3:5])#[N:4]
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참가 물질

4

반응물 2

HCID 83493Carbonochloridothioic acid, S-phenyl esterHCID 880222-Amino-2-methylpropionitrile

생성물 1

HCID 85920205(1-cyano1-methylethyl)carbamothioic acid, S-phenyl ester수율 30.6%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

3.4 g. (0.04 mole) of 2-amino-2-methylpropanonitrile are dissolved in 10 ml. of dioxane and a solution of 3.2 ml. (0.2 mole) of (phenylthio)carbonyl chloride in 10 ml. of dioxane is added. After stirring for one hour at room temperature, the reaction mixture is filtered, the filtrate is concentrated, and the solid residue is recrystallized from a small amount of toluene to yield 2.7 g of (1-cyano1-methylethyl)carbamothioic acid, S-phenyl ester; m.p. 152°-155°.

후처리

  1. filtrationthe reaction mixture is filtered
  2. concentrationthe filtrate is concentrated
  3. customthe solid residue is recrystallized from a small amount of toluene

출처 및 근거

ORD 기록
ord-f4ecdca4ae7c4dfea97c7b618470ddd7
출처 데이터셋
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04128723

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