ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Dimethylformamide → 7-bromo-N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide

HRID 1978611
ノート
印刷プレビュー

反応式

HRID 1978611 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11](=[O:13])(=[O:12])[CH2:10][CH2:9][C:8]([C:14]([OH:16])=O)=[CH:7][C:6]=2[CH:17]=1.S(Cl)(Cl)=O.CN(C=O)C.[CH3:27][N:28]([CH2:35][C:36]1[CH:42]=[CH:41][C:39]([NH2:40])=[CH:38][CH:37]=1)[CH:29]1[CH2:34][CH2:33][O:32][CH2:31][CH2:30]1>C1COCC1.C(N(CC)CC)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11](=[O:12])(=[O:13])[CH2:10][CH2:9][C:8]([C:14]([NH:40][C:39]3[CH:41]=[CH:42][C:36]([CH2:35][N:28]([CH3:27])[CH:29]4[CH2:34][CH2:33][O:32][CH2:31][CH2:30]4)=[CH:37][CH:38]=3)=[O:16])=[CH:7][C:6]=2[CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 9877845(4-Amino-benzyl)-methyl-(tetrahydro-pyran-4-yl)-amineHCID 219959787-Bromo-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid

生成物 1

HCID 219957067-bromo-N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide収率 67.5%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8471Triethylamine溶媒

実験手順

To a suspension of 7-bromo-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (4.47 g) in THF (90 ml) were added at room temperature thionyl chloride (1.03 ml) and DMF (1 ml), and the mixture was stirred for 1 hour and added dropwise to a solution of 4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]aniline (3.41 g) and triethylamine (7.9 ml) in THF (30 ml), at 0° C. The mixture was stirred for 3 hours and concentrated under reduced pressure, to which were added water. Precipitated colorless crystals were collected by filtration, and the crystals were washed with water, ethanol, 2-propanol and diisopropylether to give colorless crystals of 7-bromo-N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (4.94 g).

後処理

  1. stirringThe mixture was stirred for 3 hours
  2. concentrationconcentrated under reduced pressure, to which
  3. additionwere added water
  4. customPrecipitated colorless crystals
  5. filtrationwere collected by filtration
  6. washthe crystals were washed with water, ethanol, 2-propanol and diisopropylether

出典と根拠

ORDレコード
ord-c8f1ffe61af544ce872b7f7cdd5ea2a2
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06235771B1

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート