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Ethyl chloroformate → ethyl N-(5-ethyl-7-chloro-4,5,6,7-tetrahydrobenzothiazol-2-yl)carbamate

HRID 2058854
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HRID 2058854 반응식
[NH2:1][C:2]1[S:3][C:4]2[CH:10]([Cl:11])[CH2:9][CH:8]([CH2:12][CH3:13])[CH2:7][C:5]=2[N:6]=1.Cl[C:15]([O:17][CH2:18][CH3:19])=[O:16]>N1C=CC=CC=1>[CH2:12]([CH:8]1[CH2:7][C:5]2[N:6]=[C:2]([NH:1][C:15](=[O:16])[O:17][CH2:18][CH3:19])[S:3][C:4]=2[CH:10]([Cl:11])[CH2:9]1)[CH3:13]
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참가 물질

4

반응물 2

HCID 10928Ethyl chloroformateHCID 205484702-Amino-5-ethyl-7-chloro-4,5,6,7-tetrahydrobenzothiazole

생성물 1

HCID 20548458ethyl N-(5-ethyl-7-chloro-4,5,6,7-tetrahydrobenzothiazol-2-yl)carbamate

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

2-Amino-5-ethyl-7-chloro-4,5,6,7-tetrahydrobenzothiazole (0.10 mol) dissolved in pyridine (125 ml.) is charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and addition funnel. Ethyl chloroformate (0.12 mol) is then added dropwise to the reaction mixture with stirring and cooling. After the addition is completed the reaction mixture is allowed to warm to room temperature and stirring is continued for a period of about 1 hour. After this time the reaction mixture is poured into ice water to form a precipitate. The precipitate is recovered by filtration, is dried and recrystallized to yield the desired product ethyl N-(5-ethyl-7-chloro-4,5,6,7-tetrahydrobenzothiazol-2-yl)carbamate.

후처리

  1. additionis charged into a glass reaction vessel
  2. customequipped with a mechanical stirrer
  3. additionthermometer and addition funnel
  4. temperaturecooling
  5. additionAfter the addition
  6. stirringstirring
  7. customto form a precipitate
  8. filtrationThe precipitate is recovered by filtration
  9. customis dried
  10. customrecrystallized

출처 및 근거

ORD 기록
ord-ed63c4b7168e4621a11447da5aa85552
출처 데이터셋
uspto-grants-1982_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04319914

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