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 → [1,1'-Biphenyl]-4-carboxylic acid, 2-(phenylsulfonyl)hydrazide

HRID 393830
ノート
印刷プレビュー

反応式

HRID 393830 の反応式
[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][C:4]([C:7]([NH:9][NH2:10])=[O:8])=[CH:3][CH:2]=1.C(N(CC)C(C)C)(C)C.[C:26]1([S:32](Cl)(=[O:34])=[O:33])[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.CN(C=O)C>C1COCC1.CN(C1C=CN=CC=1)C.CCOC(C)=O>[C:26]1([S:32]([NH:10][NH:9][C:7]([C:4]2[CH:5]=[CH:6][C:1]([C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=3)=[CH:2][CH:3]=2)=[O:8])(=[O:34])=[O:33])[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 6228DimethylformamideHCID 7369Benzenesulfonyl chlorideHCID 72718p-PhenylbenzhydrazideHCID 81531Diisopropylethylamine

生成物 1

HCID 3386671[1,1'-Biphenyl]-4-carboxylic acid, 2-(phenylsulfonyl)hydrazide

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine
触媒
HCID 8028Tetrahydrofuran溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

Biphenyl-4-carboxylic acid hydrazide (0.5 g, 2.36 mmol) was suspended in THF (26 mL). N,N-diisopropylethylamine (1.64 mL, 9.44 mmol) was added, and the reaction was cooled to 0° C. Phenylsulfonyl chloride (0.33 mL, 2.59 mmol) was added followed by DMAP (5 mg, 0.04 mmol). The reaction was allowed to warm to room temperature. The solution was orange after it stirred for 1 hour; DMF (5 mL) was added, and the solution became clear. After 3 hours of stirring, the solution was diluted with EtOAc (150 mL). It was then washed with saturated sodium bicarbonate and brine and dried over Na2SO4. The reaction was then concentrated down and triturated with CH2Cl2. The desired product was isolated (0.19 g, 22.7%). MS: 351.1 (M)−1 for C19H16N2O3S); mp 216-219° C. TLC: SiO2, Rf=0.55 (1:1 hexane/EtOAc). Analysis C19H16N2O3S.0.25 H2O: (calc) C, 63.94; H, 4.66; N, 7.85. (found) C, 63.76; H, 4.64; N, 7.76. HPLC: (30% H2O/70% CH3CN/0.1% TFA), RT=3.731 min. Purity: 94.16%. IR (KBr, cm−1) 3337, 3035, 2811, 1655, 1340, 1156. 1H NMR (400 MHz, DMSO) δ 7.26-8.00 (m, 14H), 10.01 (s, 1H, 10.71 (s, 1H).

後処理

  1. temperatureto warm to room temperature
  2. stirringAfter 3 hours of stirring
  3. washIt was then washed with saturated sodium bicarbonate and brine
  4. dry with materialdried over Na2SO4
  5. concentrationThe reaction was then concentrated down
  6. customtriturated with CH2Cl2

出典と根拠

ORDレコード
ord-29629f71b44940b4b3f3aec2ca3322fd
出典データセット
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06809119B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート