Hydrochloric Acid → HCID 178477875、化合物

HRID 232850ノート

反応式

HRID 232850 の反応式
C[Sn]([N:5]=[N+:6]=[N-:7])(C)C.[Cl:8][C:9]1[CH:18]=[C:17]2[C:12]([CH:13]=[CH:14][C:15]([CH2:19][O:20][C:21]3[CH:40]=[CH:39][C:24]4[O:25][CH2:26][C:27]5[CH:38]=[CH:37][CH:36]=[CH:35][C:28]=5[CH:29]([S:30][CH2:31][CH2:32][C:33]#[N:34])[C:23]=4[CH:22]=3)=[N:16]2)=[CH:11][CH:10]=1.Cl.[OH-].[Na+]>C1(C)C(C)=CC=CC=1>[Cl:8][C:9]1[CH:18]=[C:17]2[C:12]([CH:13]=[CH:14][C:15]([CH2:19][O:20][C:21]3[CH:40]=[CH:39][C:24]4[O:25][CH2:26][C:27]5[CH:38]=[CH:37][CH:36]=[CH:35][C:28]=5[CH:29]([S:30][CH2:31][CH2:32][C:33]5[NH:34][N:7]=[N:6][N:5]=5)[C:23]=4[CH:22]=3)=[N:16]2)=[CH:11][CH:10]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 5104973Azido(trimethyl)stannaneHCID 233591442-(7-Chloroquinolin-2-yl)methoxy-11-(2-cyanoethylthio)-6,11-dihydrodibenz[b,e]oxepine

生成物 1

HCID 178477875HCID 178477875、化合物収率 4.6%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

1.25 g of trimethyltin azide was added to 1.4 g of 2-(7-chloroquinolin-2-yl)methoxy-11-(2-cyanoethylthio)-6,11-dihydrodibenz[b,e]oxepine dissolved in 40 ml of xylene and the mixture was refluxed under heating for 8.5 hours. After cooling, 1.5 ml of conc. hydrochloric acid was added to the mixture and the mixture was stirred at room temperature for 15 minutes and then adjusted to about pH 4 with a 1N-sodium hydroxide aqueous solution. Crystals precipitated were applied to silica gel column chromatography to obtain 70 mg of the title compound as light orange powder.

後処理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 8.5 hours
  3. temperatureAfter cooling
  4. customCrystals precipitated

出典と根拠

ORDレコード
ord-9c0a64eb273e4564936a45efb716099b
出典データセット
uspto-grants-1997_01
特許番号
US05591752

反応ノート

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