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Carbon Dioxide → HCID 15411537、化合物

HRID 1075378
ノート
印刷プレビュー

反応式

HRID 1075378 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 280Carbon Dioxide2 回HCID 25517Ammonium ChlorideHCID 54038012Ethyl 4-[(2-methoxyethoxy)methoxy]benzoateHCID 545731596-[(2-Methoxyethoxy)methoxy]benzothiazoleHCID 178418339Butyllithium

生成物 1

HCID 15411537HCID 15411537、化合物収率 77.8%

試薬・触媒・溶媒

3
HCID 180Acetone溶媒2 回HCID 8028Tetrahydrofuran溶媒2 回HCID 8058Hexane溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-cce432e77f514bfaba7b4c375bd3f3d9
出典データセット
uspto-grants-1999_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05900426

反応ノート

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