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Sodium Hydroxide → 7'-Bromo-4'-fluoro-2'-methoxy-5,6-dihydrospiro[[1,3]oxazine-4,9'-xanthen]-2-amine

HRID 931596
ノート
印刷プレビュー

反応式

HRID 931596 の反応式
[Br:1][C:2]1[CH:15]=[C:14]2[C:5]([O:6][C:7]3[C:8]([F:35])=[CH:9][C:10]([O:33][CH3:34])=[CH:11][C:12]=3[C:13]32[CH2:20][CH2:19][O:18][C:17]([NH:21]C(=O)C2C=CC([N+]([O-])=O)=CC=2)=[N:16]3)=[CH:4][CH:3]=1.[OH-].[Na+]>CO>[Br:1][C:2]1[CH:15]=[C:14]2[C:5]([O:6][C:7]3[C:8]([F:35])=[CH:9][C:10]([O:33][CH3:34])=[CH:11][C:12]=3[C:13]32[CH2:20][CH2:19][O:18][C:17]([NH2:21])=[N:16]3)=[CH:4][CH:3]=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

4

反応物 2

HCID 14798Sodium HydroxideHCID 67439840N-(7'-bromo-4'-fluoro-2'-methoxy-5,6-dihydrospiro[[1,3]oxazine-4,9'-xanthene]-2-yl)-4-nitrobenzamide

生成物 1

HCID 584659317'-Bromo-4'-fluoro-2'-methoxy-5,6-dihydrospiro[[1,3]oxazine-4,9'-xanthen]-2-amine収率 89.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
65 °C

実験手順

A suspension of N-(7′-bromo-4′-fluoro-2′-methoxy-5,6-dihydrospiro[[1,3]oxazine-4,9′-xanthene]-2-yl)-4-nitrobenzamide (6.0 g, 11.06 mmol) in methanol (60 mL) was heated to 65° C. NaOH (2 M solution) (48.7 ml, 97 mmol) was added and the resulting mixture was heated to 65° C. for 4 hrs. The reaction mixture was concentrated under reduced pressure, the precipitate was filtered off, washed twice with water and dried to afford 7′-bromo-4′-fluoro-2′-methoxy-5,6-dihydrospiro[[1,3]oxazine-4,9′-xanthen]-2-amine (3.90 g, 9.92 mmol, 50.9% yield) as white solid.

後処理

  1. temperaturethe resulting mixture was heated to 65° C. for 4 hrs
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. filtrationthe precipitate was filtered off
  4. washwashed twice with water
  5. customdried

出典と根拠

ORDレコード
ord-50bf43408fba4d63a6c7661dcebd9470
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296759B2

反応ノート

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