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

HRID 2252264
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HRID 2252264 반응식
[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]
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참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

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온도
0 °C

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-6ea6c9cf8bcd4b9784b649edc9b3d2c8
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07320986B2

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