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2-Dimethylaminopyridine → HCID 68914455, 화합물

HRID 870379
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HRID 870379 반응식
[C:1]([O:5][C:6](=[O:22])[N:7]([C@H:11]1[CH2:20][CH2:19][C:18]2[C:13](=[CH:14][CH:15]=[C:16]([NH2:21])[CH:17]=2)[CH2:12]1)[CH2:8][CH2:9][CH3:10])([CH3:4])([CH3:3])[CH3:2].CN(C1C=CC=CN=1)C.[F:32][C:33]([F:46])([F:45])[CH2:34][C:35]1[CH:40]=[CH:39][C:38]([S:41](Cl)(=[O:43])=[O:42])=[CH:37][CH:36]=1>O1CCCC1>[C:1]([O:5][C:6](=[O:22])[N:7]([CH2:8][CH2:9][CH3:10])[C@H:11]1[CH2:20][CH2:19][C:18]2[C:13](=[CH:14][CH:15]=[C:16]([NH:21][S:41]([C:38]3[CH:37]=[CH:36][C:35]([CH2:34][C:33]([F:32])([F:45])[F:46])=[CH:40][CH:39]=3)(=[O:43])=[O:42])[CH:17]=2)[CH2:12]1)([CH3:2])([CH3:3])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 218852-DimethylaminopyridineHCID 536286074-(2,2,2-Trifluoroethyl)benzene-1-sulfonyl chlorideHCID 68914769HCID 68914769, 화합물

생성물 1

HCID 68914455HCID 68914455, 화합물수율 97.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

((S)-6-Amino-1,2,3,4-tetrahydro-naphthalen-2-yl)-propyl-carbamic acid tert-butyl ester (720 mg, 2.37 mmol) was dissolved in tetrahydrofurane (50 ml). Then, dimethylamino pyridine (100 mg, 0.82 mmol) and 4-(2,2,2-trifluoro-ethyl)benzenesulfonyl chloride (761 mg, 2.37 mmol) were added and the reaction mixture was stirred for 30 minutes at room temperature. The solvent was evaporated under reduced pressure, the residue treated with water and diethyl ether. The organic layer was dried over magnesium sulfate, filtered, and the solvent evaporated under reduced pressure to give the crude product (1.22 g, 95% purity, 93% yield).

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. additionthe residue treated with water and diethyl ether
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. customthe solvent evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-4a90f03b72ff478db7a53dcf37745e63
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969552B2

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