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Triphenylphosphine → 4-((4-(Difluoromethyl)-1,3-thiazol-2-yl)methoxy)-1-(2-ethyl-1-methyl-1H-benzimidazol-6-yl)pyridin-2(1H)-one

HRID 2203111
ノート
印刷プレビュー

反応式

HRID 2203111 の反応式
[F:1][CH:2]([F:10])[C:3]1[N:4]=[C:5]([CH2:8][OH:9])[S:6][CH:7]=1.[CH2:11]([C:13]1[N:17]([CH3:18])[C:16]2[CH:19]=[C:20]([N:23]3[CH:28]=[CH:27][C:26](O)=[CH:25][C:24]3=[O:30])[CH:21]=[CH:22][C:15]=2[N:14]=1)[CH3:12].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCCOC)=O)=NC(OCCOC)=O>O.C1COCC1>[F:1][CH:2]([F:10])[C:3]1[N:4]=[C:5]([CH2:8][O:9][C:26]2[CH:27]=[CH:28][N:23]([C:20]3[CH:21]=[CH:22][C:15]4[N:14]=[C:13]([CH2:11][CH3:12])[N:17]([CH3:18])[C:16]=4[CH:19]=3)[C:24](=[O:30])[CH:25]=2)[S:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 11776TriphenylphosphineHCID 533844152-methoxyethyl N-(2-methoxyethoxycarbonylimino)carbamateHCID 680963792-Thiazolemethanol, 4-(difluoromethyl)-HCID 896909981-(2-Ethyl-1-methyl-1H-benzimidazol-6-yl)-4-hydroxypyridin-2(1H)-one

生成物 1

HCID 897026674-((4-(Difluoromethyl)-1,3-thiazol-2-yl)methoxy)-1-(2-ethyl-1-methyl-1H-benzimidazol-6-yl)pyridin-2(1H)-one
収率 13.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of (4-(difluoromethyl)-1,3-thiazol-2-yl)methanol (61.3 mg), 1-(2-ethyl-1-methyl-1H-benzo[d]imidazol-6-yl)-4-hydroxypyridin-2(1H)-one (50 mg), triphenylphosphine (146 mg), bis(2-methoxyethyl) azodicarboxylate (130 mg) and THF (3 ml) was stirred at room temperature for 3 h. The mixture was diluted with water, and extracted with EtOAc. The extract was washed with brine, dried over MgSO4, concentrated in vacuo and purified by NH silica gel column chromatography (hexane/EtOAc) to give the title compound (10.1 mg) as a white solid.

後処理

  1. extractionextracted with EtOAc
  2. washThe extract was washed with brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. custompurified by NH silica gel column chromatography (hexane/EtOAc)

出典と根拠

ORDレコード
ord-9ee8129c1882422a8895680434487701
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09365540B2

反応ノート

読み込み中…

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