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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
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Water → HCID 10621601、化合物

HRID 1031712
ノート
印刷プレビュー

反応式

HRID 1031712 の反応式
[CH3:1][S:2]([NH:5][C:6]1[C:16]([O:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[CH:15][C:9]2[C:10](=[O:14])[CH2:11][CH2:12][O:13][C:8]=2[CH:7]=1)(=[O:4])=[O:3].[Br:24]Br.O>C(Cl)(Cl)Cl>[Br:24][CH:11]1[C:10](=[O:14])[C:9]2[CH:15]=[C:16]([O:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:6]([NH:5][S:2]([CH3:1])(=[O:3])=[O:4])=[CH:7][C:8]=2[O:13][CH2:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 24408BromineHCID 10806538HCID 10806538、化合物

生成物 1

HCID 10621601HCID 10621601、化合物収率 97.4%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

In 300 ml of chloroform was dissolved 33.3 g of 2,3-dihydro-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one. To this solution being maintained at 25°-30° C. was dropwise added 16.3 g of bromine in 30 minutes. After the completion of the dropwise addition, the mixture was stirred for 30 minutes at 25°-30° C. 100 ml of water was added thereto. The organic layer was separated, washed with a 5% aqueous sodium thiosulfate solution, water and a saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure to obtain 40.1 g (yield: 97.3%) of 3-bromo-2,3-dihydro-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one.

後処理

  1. temperatureTo this solution being maintained at 25°-30° C.
  2. customin 30 minutes
  3. additionAfter the completion of the dropwise addition
  4. customThe organic layer was separated
  5. washwashed with a 5% aqueous sodium thiosulfate solution, water
  6. dry with materiala saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate
  7. customThe solvent was removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-04e36da916864fcd850abd73732c0508
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04954518

反応ノート

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