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Acetic Acid → HCID 178519127, 화합물

HRID 1909493
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HRID 1909493 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@H:8]2[CH2:13][CH2:12][C@H:11]([CH:14]=O)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C(O)(=O)C.[C:20]1(=[O:31])[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=2[C:23](=[O:30])[CH2:22][O:21]1.N1CCOCC1>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C@H:8]2[CH2:9][CH2:10][C@H:11](/[CH:14]=[C:22]3\[O:21][C:20](=[O:31])[C:25]4[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=4[C:23]\3=[O:30])[CH2:12][CH2:13]2)=[CH:6][CH:7]=1
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참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 8083MorpholineHCID 126956791H-2-Benzopyran-1,4(3H)-dioneHCID 178520920HCID 178520920, 화합물

생성물 1

HCID 178519127HCID 178519127, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
40 °C

실험 절차

To the resulting stirred mixture from stage 1, at ambient temperature under argon, was added acetic acid (250 mL), 1H-2-benzopyran-1,4(3H)-dione (compound of formula (III)) (32.4 g, 200 mmol) and morpholine (17.5 mL, 200 mmol). The reaction mixture was heated to 40° C. for 4 hours then allowed to cool to ambient temperature and stir overnight. Water (250 mL) was added and the slurry stirred for 15 minutes at ambient temperature then filtered. The filter cake was washed twice with tert-butyl methyl ether (2×125 mL) and dried to give the title compound as a yellow solid (62.4 g). The material obtained was spectroscopically identical to that obtained in Stage 2, Example 3.

후처리

  1. temperatureto cool to ambient temperature
  2. stirringthe slurry stirred for 15 minutes at ambient temperature
  3. filtrationthen filtered
  4. washThe filter cake was washed twice with tert-butyl methyl ether (2×125 mL)
  5. customdried

출처 및 근거

ORD 기록
ord-468385e9c4ce47c5adcdaf789558130a
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598387B2

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