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Carbon Dioxide → HCID 15411537, 화합물

HRID 1075378
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HRID 1075378 반응식
C([Li])CCC.[CH3:6][O:7][CH2:8][CH2:9][O:10][CH2:11][O:12][C:13]1[CH:21]=[CH:20][C:16]2[N:17]=[CH:18][S:19][C:15]=2[CH:14]=1.C(=O)=O.[CH3:25][O:26][CH2:27][CH2:28][O:29][CH2:30][O:31][C:32]1[CH:42]=[CH:41][C:35]([C:36](OCC)=[O:37])=[CH:34][CH:33]=1.[NH4+].[Cl-]>CCCCCC.O1CCCC1.CC(C)=O>[CH3:6][O:7][CH2:8][CH2:9][O:10][CH2:11][O:12][C:13]1[CH:21]=[CH:20][C:16]2[N:17]=[C:18]([C:36](=[O:37])[C:35]3[CH:34]=[CH:33][C:32]([O:31][CH2:30][O:29][CH2:28][CH2:27][O:26][CH3:25])=[CH:42][CH:41]=3)[S:19][C:15]=2[CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 280Carbon Dioxide2회HCID 25517Ammonium ChlorideHCID 54038012Ethyl 4-[(2-methoxyethoxy)methoxy]benzoateHCID 545731596-[(2-Methoxyethoxy)methoxy]benzothiazoleHCID 178418339Butyllithium

생성물 1

HCID 15411537HCID 15411537, 화합물수율 77.8%

시약·촉매·용매

3
HCID 180Acetone용매2회HCID 8028Tetrahydrofuran용매2회HCID 8058Hexane용매

실험 절차

A solution of 1.3 N of n-butyllithium in hexane (0.7 ml) was added to a solution of 220 mg of 6-[(2-methoxyethoxy)methoxy]benzothiazole (obtained as in paragraph 1 above) in 30 ml of tetrahydrofuran at -78° C. cooled by dry ice--acetone. The mixture was added dropwise into a solution of 234 mg of ethyl 4-[(2-methoxyethoxy)methoxy]benzoate (obtained as in paragraph 2 above) in tetrahydrofuran (3 ml) cooled by dry ice--acetone. NH4Cl was added to the reaction mixture and the mixture was extracted with ether. The extracts were washed with water and dried over sodium sulfate. After being concentrated, the residue was recrystallized from ethyl acetate to yield 320 mg of 6-(2-methoxyethoxy)methoxy-2-{4-[(2-methoxyethoxy)methoxy]benzoyl}benzothiazole (Compound 1). mp: 46° C. 1H-NMR(CDCl3): 3.38(s,3H), 3.38(s,3H), 3.58(m,4H), 3.86(m,4H), 5.38(s,4H), 7.18(d,J=8.8 Hz,2H), 7.28(dd,J=9.1,2.2 Hz,1H), 7.67(d,J=2.2 Hz,1H), 8.10(d,J=9.1 Hz,1H), 8.59(d,J=8.8 Hz,2H) IR(KBr) cm-1 : 2877, 1598, 1488, 1214, 1117, 987 MS m/z: 447(M+), 89, 59 Elementary analysis (C22H25NO7S): Calculated (C=59.05,H=5.63,N=3.13); Found (C=59.15,H=5.58,N=2.93)

후처리

  1. extractionthe mixture was extracted with ether
  2. washThe extracts were washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationAfter being concentrated
  5. customthe residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-cce432e77f514bfaba7b4c375bd3f3d9
출처 데이터셋
uspto-grants-1999_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05900426

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