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Ethyl Acetate → HCID 178496377, 화합물

HRID 1695591
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인쇄 미리보기

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HRID 1695591 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:11]=1[CH:10]([NH:12][C:13]1[O:14][CH2:15][C:16]3[CH:22]=[C:21]([NH2:23])[CH:20]=[CH:19][C:17]=3[N:18]=1)[CH2:9]C2.[CH3:24][O:25][CH2:26][C:27](Cl)=[O:28].C(OCC)(=[O:32])C>C(=O)([O-])O.[Na+]>[CH3:24][O:25][CH2:26][C:27]([NH:23][C:21]1[CH:20]=[CH:19][C:17]2[N:18]=[C:13]([NH:12][CH:10]3[C:11]4[C:3]([O:2][CH3:1])=[CH:4][CH:5]=[CH:6][C:7]=4[O:32][CH2:9]3)[O:14][CH2:15][C:16]=2[CH:22]=1)=[O:28]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8857Ethyl Acetate2회HCID 96623Methoxyacetyl chlorideHCID 178488335HCID 178488335, 화합물

생성물 1

HCID 178496377HCID 178496377, 화합물수율 73%

시약·촉매·용매 1

HCID 516892Sodium Bicarbonate용매

반응 조건

온도
23 °C

실험 절차

To a solution of rac-N2-(7-methoxy-indan-1-yl)-4H-benzo[d][1,3]oxazine-2,6-diamine (Example 10) (100 mg, 0.321 mmol) in ethyl acetate (5 ml) and sat. sodium hydrogen carbonate-sol. at 0° C. was added methoxyacetyl chloride (35 ul, 0.385 mmol) and the mixture was stirred at 23° C. for 16 h. Diluted with ethyl acetate, washed with water, dried the organic layer over sodium sulfate. After filtration, the solvent was removed in vacuum and the crude product was triturated with diethyl ether to give the title compound as a white solid (90 mg, 73%), MS (ISP) m/e=384.2 [(M+H)+].

후처리

  1. washwashed with water
  2. dry with materialdried the organic layer over sodium sulfate
  3. filtrationAfter filtration
  4. customthe solvent was removed in vacuum
  5. customthe crude product was triturated with diethyl ether

출처 및 근거

ORD 기록
ord-bfd3456c1e7241d1bd3f1d0a4da9ab5f
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163740B2

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