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Butanedioic acid, 2,3-dihydroxy-, diethyl ester, S-(R*,R*)- → HCID 10293318、化合物

HRID 1816675
ノート
印刷プレビュー

反応式

HRID 1816675 の反応式
[F:1][C:2]([F:25])([F:24])[CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([CH2:13][S:14][C:15]2[NH:19][C:18]3[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=3[N:16]=2)[CH:8]=1.C(C(C(C(OCC)=O)O)O)(OCC)=[O:27].C(N(CC)C(C)C)(C)C.OOOO.C1(C(C)C)C=CC=CC=1.C(=O)(O)[O-].[Na+]>C(OCC)(=O)C.CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4].O>[F:25][C:2]([F:24])([F:1])[CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([CH2:13][S:14]([C:15]2[NH:16][C:17]3[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=3[N:19]=2)=[O:27])[CH:8]=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 62333Butanedioic acid, 2,3-dihydroxy-, diethyl ester, S-(R*,R*)-HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 21889389HCID 21889389、化合物HCID 22493631HCID 22493631、化合物

生成物 1

HCID 10293318HCID 10293318、化合物

試薬・触媒・溶媒 3

HCID 11026Titanium isopropoxide触媒
HCID 962Water溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

2-[4-(4,4,4-Trifluorobutoxy)pyridin-2-yl-methylthio]-1H-benzimidazole (6.0 g) was dissolved in ethyl acetate (150 mL). Molecular Sieve 4A (6.0 g) and water (290 μL) were added, and the mixture was stirred for 15 minutes at room temperature. Subsequently, diethyl (+)-tartrate (6.7 g) and tetraisopropyl titanate (4.6 g) were added, and the mixture was stirred for one hour at 50° C. The temperature of the mixture was returned to room temperature. N,N-Diisopropylethylamine (2.8 mL) and 88% cumene hydroxyperoxide (2.7 mL) were added, and the mixture was stirred for four hours at room temperature. A saturated sodium bicarbonate solution was added to the reaction mixture, and the mixture was stirred for 30 minutes, followed by filtration through the Celite. The filtrate was extracted with ethyl acetate. The organic layer was washed sequentially with water and brine, and brought to dryness over sodium sulfate anhydrate. The solvent was removed under reduced pressure. The residue was subjected to silica gel column chromatography (silica gel: NH-DM1020 (product of Fuji Silicia), chloroform:methanol=10:1), whereby (−)-2-[4-(4,4,4-trifluorobutoxy) pyridin-2-yl-methanesulfinyl]-1H-benzimidazole was obtained (4.5 g).

後処理

  1. stirringthe mixture was stirred for one hour at 50° C
  2. customwas returned to room temperature
  3. stirringthe mixture was stirred for four hours at room temperature
  4. stirringthe mixture was stirred for 30 minutes
  5. filtrationfollowed by filtration through the Celite
  6. extractionThe filtrate was extracted with ethyl acetate
  7. washThe organic layer was washed sequentially with water and brine
  8. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-6518ab0ad6f8432a8c561c9d70d008ac
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06884810B2

反応ノート

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