Toluene → Ethyl 2-[6-fluoro-3-(2-propenyl)-2(3H)-benzothiazolon-5-ylaminocarbonyl]-hexahydropyridazine-1-carboxylate

HRID 1199144ノート

反応式

HRID 1199144 の反応式
[F:1][C:2]1[C:14]([N:15]=[C:16]=[O:17])=[CH:13][C:5]2[N:6]([CH2:10][CH:11]=[CH2:12])[C:7](=[O:9])[S:8][C:4]=2[CH:3]=1.[N:18]1([C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:23][CH2:22][CH2:21][CH2:20][NH:19]1.C1(C)C=CC=CC=1.C(N(CC)CC)C>O>[F:1][C:2]1[C:14]([NH:15][C:16]([N:19]2[CH2:20][CH2:21][CH2:22][CH2:23][N:18]2[C:24]([O:26][CH2:27][CH3:28])=[O:25])=[O:17])=[CH:13][C:5]2[N:6]([CH2:10][CH:11]=[CH2:12])[C:7](=[O:9])[S:8][C:4]=2[CH:3]=1

参加物

6

反応物 4

HCID 1140TolueneHCID 8471TriethylamineHCID 30143771(2H)-Pyridazinecarboxylic acid, tetrahydro-, ethyl esterHCID 143064846-Fluoro-3-(2-propenyl)-2(3H)-benzothiazolon-5-yl isocyanate

生成物 1

HCID 14049866Ethyl 2-[6-fluoro-3-(2-propenyl)-2(3H)-benzothiazolon-5-ylaminocarbonyl]-hexahydropyridazine-1-carboxylate収率 69.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

6-Fluoro-3-(2-propenyl)-2(3H)-benzothiazolon-5-yl isocyanate (1.99 g) and ethyl hexahydropyridazine-1-carboxylate (1.26 g) were added to toluene (8 ml). A catalytic amount of triethylamine was added thereto, and the resultant mixture was stirred at 25° C. for 12 hours. Water was added thereto, and the resultant mixture was extracted with toluene. The extract was washed with water, dried and concentrated to give ethyl 2-[6-fluoro-3-(2-propenyl)-2(3H)-benzothiazolon-5-ylaminocarbonyl]-hexahydropyridazine-1-carboxylate (2.26 g). m.p., 161.2° C.

後処理

  1. extractionthe resultant mixture was extracted with toluene
  2. washThe extract was washed with water
  3. customdried
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-23f81fb8ddea4d6fb93a69cfaa2dbcfc
出典データセット
uspto-grants-1990_02
特許番号
US04898948

反応ノート

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