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Hydrochloric Acid → 4-(2-Carbamoyl-2-cyano-thioacetylamino)-benzoic acid t-butyl ester

HRID 1993826
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HRID 1993826 반응식
[C:1]([O:5][C:6](=[O:16])[C:7]1[CH:12]=[CH:11][C:10]([N:13]=[C:14]=[S:15])=[CH:9][CH:8]=1)([CH3:4])([CH3:3])[CH3:2].[OH-].[K+].[C:19]([CH2:21][C:22]([NH2:24])=[O:23])#[N:20].Cl>CN(C=O)C>[C:1]([O:5][C:6](=[O:16])[C:7]1[CH:8]=[CH:9][C:10]([NH:13][C:14](=[S:15])[CH:21]([C:22](=[O:23])[NH2:24])[C:19]#[N:20])=[CH:11][CH:12]=1)([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7898CyanoacetamideHCID 14797Potassium HydroxideHCID 4281352tert-Butyl 4-isothiocyanatobenzoate

생성물 1

HCID 597976494-(2-Carbamoyl-2-cyano-thioacetylamino)-benzoic acid t-butyl ester수율 83.5%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

4-Isothiocyanato-benzoic acid t-butyl ester 2 (28.3 gm, 120.4 mmol) was taken into DMF (200 ml). To this KOH (6.74 gm, 120.4 mmol) and cyanoacetamide (10.21 gm, 120.4 mmol) were added. The reaction mixture was stirred at room temperature for 16 h. The reaction mixture was acidified with 1N HCl, the precipitate obtained was filtered, washed with water, and dried under vacuum, to provide 32.10 gm of 4-(2-Carbamoyl-2-cyano-thioacetylamino)-benzoic acid t-butyl ester 3.

후처리

  1. customthe precipitate obtained
  2. filtrationwas filtered
  3. washwashed with water
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-136e7af863204f16940d7a3a7e878f9e
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07652047B2

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