Triethylamine → 6-Methyl-2-(1-oxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)quinazolin-4(3H)-one

HRID 540218ノート

反応式

HRID 540218 の反応式
Cl[C:2]1[NH:11][C:10](=[O:12])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([CH3:13])[CH:8]=2)[N:3]=1.[S:14]1(=[O:25])[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[CH2:18][NH:17][CH2:16][CH2:15]1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH3:13][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[N:3]=[C:2]([N:17]1[CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[S:14](=[O:25])[CH2:15][CH2:16]1)[NH:11][C:10]2=[O:12]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 196082032,3,4,5-Tetrahydrobenzo[f][1,4]thiazepine 1-oxideHCID 1355887902-Chloro-6-methyl-3,4-dihydroquinazolin-4-one

生成物 1

HCID 1363367986-Methyl-2-(1-oxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)quinazolin-4(3H)-one収率 80%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a stirred solution of 2-chloro-6-methylquinazolin-4(3H)-one (15 g, 77.3 mmol) and 2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide (16.8 g, 103 mmol) in toluene (200 mL) was added triethylamine (16.1 mL, 116 mmol). After being refluxed overnight, the reaction mixture was cooled to room temperature. The formed solid was collected by filtration, washed with ethanol (50 mL) and ethyl acetate (100 mL), and then dried in vacuo to afford 21.0 g of the desired product as a white solid (yield was 80%).

後処理

  1. temperatureAfter being refluxed overnight
  2. filtrationThe formed solid was collected by filtration
  3. washwashed with ethanol (50 mL) and ethyl acetate (100 mL)
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-59da41b5036a4b53a61f068805f8a67a
出典データセット
uspto-grants-2014_10
特許番号
US08871756B2

反応ノート

読み込み中…