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Isobutylene → HCID 22241519, 화합물

HRID 892220
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인쇄 미리보기

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HRID 892220 반응식
[CH3:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([CH2:10][O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH2:19][C:20]3[N:29]([CH3:30])[C:28](=[O:31])[C:27]4[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=4)[N:21]=3)[CH:13]=2)[C:3]=1[CH:4]=[O:5].C=C(C)C.[O-:36]Cl=O.[Na+]>C(O)(C)(C)C.O.C(OCC)(=O)C>[CH3:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([CH2:10][O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH2:19][C:20]3[N:29]([CH3:30])[C:28](=[O:31])[C:27]4[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=4)[N:21]=3)[CH:13]=2)[C:3]=1[C:4]([OH:36])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 8255IsobutyleneHCID 22241385HCID 22241385, 화합물HCID 23668197Sodium Chlorite

생성물 1

HCID 22241519HCID 22241519, 화합물

시약·촉매·용매 3

HCID 962Water용매2회HCID 6386tert-Butanol용매
HCID 8857
Ethyl Acetate
용매

실험 절차

To a suspension of 2-methyl-6-[3-(3-methyl-4-oxo-3,4-dihydro-quinazolin-2-ylmethoxy)phenoxymethyl]-benzaldehyde (120 mg, 0.28 mmol, example 102) in t-butanol (1.5 mL) is added iso-butene (0.5 mL) followed by NaClO2 (220 mg, tech grade 1.6 mmol) in water (1.5 mL) and NaH2PO4.H2O (220 mg, 1.6 mmol) in water (1.5 mL). This mixture is stirred for 1 h (during which time the solids dissolve) then diluted with ethyl acetate, washed with water and brine, dried over MgSO4 and concentrated. The residue is purified by flash chromatography (10% methanol in dichloromethane). This product was suspended in chloroform and filtered through celite. The filtrate is concentrated under reduced pressure to give the title compound as an amorphous solid. 1H NMR (300 MHz, CDCl3): δ 8.41 (d, 1H), 7.84 (m, 2H), 7.62 (m, 1H), 7.33 (m, 2H), 7.20 (m, 1H), 7.14 (t, 1H), 6.81 (m, 1H), 6.70 (m, 2H), 5.29 (s, 2H), 5.25 (s, 2H), 3.80 (s, 2H), 2.52 (s, 3H). MS (ESI) 430 (M+H)+.

후처리

  1. dissolutiondissolve)
  2. washwashed with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe residue is purified by flash chromatography (10% methanol in dichloromethane)
  6. filtrationfiltered through celite
  7. concentrationThe filtrate is concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-cebfbb389a2446498303c224f86b6a77
출처 데이터셋
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07005440B1

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