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Sodium Cyanate → [4-(3'-Chloro-2-fluoro-6-methoxy-biphenyl-3-ylmethyl)-phenyl]-urea

HRID 1632032
ノート
印刷プレビュー

反応式

HRID 1632032 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[C:13]([O:14][CH3:15])=[CH:12][CH:11]=[C:10]([CH2:16][C:17]3[CH:22]=[CH:21][C:20]([NH2:23])=[CH:19][CH:18]=3)[C:9]=2[F:24])[CH:5]=[CH:6][CH:7]=1.[O-:25][C:26]#[N:27].[Na+].CC(C)=O.CCCCCC>CC(O)=O.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[C:13]([O:14][CH3:15])=[CH:12][CH:11]=[C:10]([CH2:16][C:17]3[CH:18]=[CH:19][C:20]([NH:23][C:26]([NH2:27])=[O:25])=[CH:21][CH:22]=3)[C:9]=2[F:24])[CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 517096Sodium CyanateHCID 21880519Acetone hexaneHCID 580200234-(3'-Chloro-2-fluoro-6-methoxy-biphenyl-3-ylmethyl)-phenylamine

生成物 1

HCID 46213059[4-(3'-Chloro-2-fluoro-6-methoxy-biphenyl-3-ylmethyl)-phenyl]-urea収率 56%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒
HCID 962
Water
溶媒
2 回

実験手順

A mixture of 4-(3′-chloro-2-fluoro-6-methoxy-biphenyl-3-ylmethyl)-phenylamine (I-35) (100 mg, 0.26 mmol, 1 eq.), sodium cyanate (74 mg, 0.52 mmol, 2 eq.) in HOAc (1 ml) and water (1 ml) was sonicated at rt for 20 min. then was shaken at rt overnight. The mixture was diluted with water. The precipitate was collected by filtration and washed with water. After dried, 71 mg of crude product containing a less polar by product (presumably the corresponding acetamide) was obtained. Trituration of the crude product with acetone/hexane gave 56 mg of [4-(3′-chloro-2-fluoro-6-methoxy-biphenyl-3-ylmethyl)-phenyl]-urea (P-243) as white solid in 56% yield. 1H NMR (DMSO-d6, 400 MHz): 8.42 (s, 1H), 7.40-7.47 (m, 2H), 7.36 (m, 1H), 7.23-7.32 (m, 4H), 7.07 (m, 2H), 6.92 (m, 1H), 5.76 (s, 2H), 3.83 (s, 2H), 3.72 (s, 3H) ppm.

後処理

  1. customwas sonicated at rt for 20 min.
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with water
  4. customAfter dried
  5. addition71 mg of crude product containing a less polar by product (presumably the corresponding acetamide)
  6. customwas obtained

出典と根拠

ORDレコード
ord-b15e265d93554cc1a043e8d2a4f5088b
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08791267B2

反応ノート

読み込み中…

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