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Dimethylamine → HCID 57722500, 화합물

HRID 1986619
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HRID 1986619 반응식
[CH3:1][NH:2][S:3]([C:6]1[CH:15]=[CH:14][C:13]2[CH2:12][CH2:11][C:10](=[O:16])[CH2:9][C:8]=2[CH:7]=1)(=[O:5])=[O:4].N(C)[CH3:18]>C(Cl)Cl>[CH3:1][N:2]([CH3:18])[S:3]([C:6]1[CH:15]=[CH:14][C:13]2[CH2:12][CH2:11][C:10](=[O:16])[CH2:9][C:8]=2[CH:7]=1)(=[O:4])=[O:5]
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참가 물질

4

반응물 2

HCID 674DimethylamineHCID 57722504HCID 57722504, 화합물

생성물 1

HCID 57722500HCID 57722500, 화합물수율 45%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 7-oxo-5,6,7,8-tetrahydro-naphthalene-2-sulfonyl chloride (see Preparative Example 3, 1.0 g, 4.1 mmol) in CH2Cl2 (10 mL) at 15° C. (using a water bath) was added Me2NH (2M in THF, 8 mL, 16 mmol, 4 eq) dropwise. After stirring at room temperature for 30 minutes, the mixture was diluted with CH2Cl2 (30 mL), washed with H2O (20 mL), dried (Na2SO4), and concentrated. The residue was chromatographed on silica using 20% EtOAc/hexanes to give 0.46 g (45%) of 7-oxo-5,6,7,8-tetrahydro-naphthalene-2-sulfonic acid dimethylamide as a yellow oil. 1H NMR (300 MHz, CDCl3): δ 7.61 (d, 1H, J=8.1 Hz), 7.53 (s, 1H), 7.41 (d, 1H, J=8.1 Hz), 3.65 (s, 2H), 3.14 (t, 2H, J=6.6 Hz), 2.71 (s, 6H), 2.58 (t, 2H, J=6.6 Hz).

후처리

  1. washwashed with H2O (20 mL)
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated
  4. customThe residue was chromatographed on silica using 20% EtOAc/hexanes

출처 및 근거

ORD 기록
ord-c9007ce84fc647459e756b2f4c3cf16c
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07550467B2

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