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O-Ethyl carbamothioate → 2-Hydroxy-5,6-dihydro-4H-benzothiazol-7-one

HRID 1580089
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HRID 1580089 반응식
Cl[CH:2]1[C:7](=O)[CH2:6][CH2:5][CH2:4][C:3]1=[O:9].[C:10](=[S:15])([O:12]CC)[NH2:11]>O>[O:9]=[C:3]1[C:2]2[S:15][C:10](=[O:12])[NH:11][C:7]=2[CH2:6][CH2:5][CH2:4]1
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참가 물질

4

반응물 2

HCID 3032339O-Ethyl carbamothioateHCID 134833282-Chloro-1,3-cyclohexanedione

생성물 1

HCID 64245982-Hydroxy-5,6-dihydro-4H-benzothiazol-7-one수율 36.1%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
140 °C

실험 절차

A mixture of 29.3 g of 2-chloro-1,3-cyclohexanedione [Muehlstaedt et al, J. Prakt Chem., Vol. 20 (1963), p. 285] and 21 g of ethyl thiocarbamate was heated at 140°C for 15 minutes and was then poured into water. The precipitate formed was recovered by vacuum filtering and was crystallized from isopropyl alcohol to obtain 12.2 g of 7-oxo-2,3,4,5,6,7-hexahydrobenzothiazoline-2-one melting at 262°C.

후처리

  1. customThe precipitate formed
  2. customwas recovered by vacuum
  3. filtrationfiltering
  4. customwas crystallized from isopropyl alcohol

출처 및 근거

ORD 기록
ord-9a294540aabe4ec2b63d58a707f0442b
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03932433

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