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

HRID 2058851노트

반응식

HRID 2058851 반응식
[NH2:1][C:2]1[S:3][C:4]2[C:10]([CH3:12])([CH3:11])[CH2:9][C:8]([CH3:14])([CH3:13])[CH2:7][C:5]=2[N:6]=1.Cl[C:16]([O:18][CH2:19][CH3:20])=[O:17]>N1C=CC=CC=1>[CH3:13][C:8]1([CH3:14])[CH2:7][C:5]2[N:6]=[C:2]([NH:1][C:16](=[O:17])[O:18][CH2:19][CH3:20])[S:3][C:4]=2[C:10]([CH3:12])([CH3:11])[CH2:9]1

참가 물질

4

반응물 2

HCID 10928Ethyl chloroformateHCID 127833484,5,6,7-tetrahydro-5,5,7,7-tetramethyl-2-Benzothiazolamine

생성물 1

HCID 20548456Ethyl N-(5,5,7,7-Tetramethyl-4,5,6,7-tetrahydrobenzothiazol-2-yl)carbamate

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

2-Amino-5,5,7,7-tetramethyl-4,5,6,7-tetrahydrobenzothiazole (16 grams; 0.075 mol) dissolved in pyridine (100 ml) was charged into a glass reaction vessel equipped with a mechanical stirrer and addition funnel. Ethyl chloroformate (11 grams; 0.1 mol) was then added dropwise with stirring and cooling of the reaction mixture. After the addition was completed the reaction mixture was allowed to warm to room temperature and stirring was continued for a period of about 1 hour. After this time the reaction mixture was poured into ice water resulting in a white precipitate. The precipitate was recovered by filtration, was dried and recrystallized from methanol to yield the desired product ethyl N-(5,5,7,7-tetramethyl-4,5,6,7-tetrahydrobenzothiazol-2-yl) carbamate having a melt point of 124° to 125° C.

후처리

  1. additionwas charged into a glass reaction vessel
  2. customequipped with a mechanical stirrer and addition funnel
  3. temperaturecooling of the reaction mixture
  4. additionAfter the addition
  5. stirringstirring
  6. filtrationThe precipitate was recovered by filtration
  7. customwas dried
  8. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-84f411cbf742456bba4adb9342980d89
출처 데이터셋
uspto-grants-1982_03
특허 번호
US04319914

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