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

HRID 2058851ノート

反応式

HRID 2058851 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-84f411cbf742456bba4adb9342980d89
出典データセット
uspto-grants-1982_03
特許番号
US04319914

反応ノート

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