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Ammonia → (1-Oxo-2,3-dihydro-1h-inden-5-yl)methyl methanesulfonate

HRID 2252264
ノート
印刷プレビュー

反応式

HRID 2252264 の反応式
[OH:1][CH2:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[CH2:7][CH2:6]2.C(N(CC)CC)C.[CH3:20][S:21](Cl)(=[O:23])=[O:22].N>O1CCCC1.O>[CH3:20][S:21]([O:1][CH2:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[CH2:7][CH2:6]2)(=[O:23])=[O:22]
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

7

反応物 4

HCID 222AmmoniaHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 691985325-(Hydroxymethyl)-2,3-dihydro-1H-inden-1-one

生成物 1

HCID 85997625(1-Oxo-2,3-dihydro-1h-inden-5-yl)methyl methanesulfonate

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
0 °C

実験手順

To a mixture of Example 332C (3.8 g, 23.6 mmol) and triethylamine (4.3 mL, 30.7 mmol) in tetrahydrofuran (50 mL) was added methanesulfonyl chloride (2.2 mL, 28.3 mmol) dropwise at about 0° C. After about 30 min stirring at about 0° C., the reaction mixture was diluted with water and was extracted with ethyl acetate. The combined organic extracts were washed with brine, dried (MgSO4), filtered and evaporated under reduced pressure to give the above intermediate. MS (DCI/NH3): m/z 258 (M+NH4)+.

後処理

  1. extractionwas extracted with ethyl acetate
  2. washThe combined organic extracts were washed with brine
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customto give the above intermediate

出典と根拠

ORDレコード
ord-6ea6c9cf8bcd4b9784b649edc9b3d2c8
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07320986B2

反応ノート

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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