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Ammonium Acetate → HCID 178433035、化合物

HRID 549352
ノート
印刷プレビュー

反応式

HRID 549352 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]([C:16]2[N:17]=[C:18]([CH3:28])[S:19][C:20]=2[C:21]2[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=2)=[O:15])[CH:10]([CH2:29][C:30](OCC(C2C=CC(F)=CC=2)=O)=O)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[C:43]([O-])(=O)[CH3:44].[NH4+:47]>>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]([C:16]2[N:17]=[C:18]([CH3:28])[S:19][C:20]=2[C:21]2[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=2)=[O:15])[CH:10]([CH2:29][C:30]2[NH:47][CH:10]=[C:9]([C:43]3[CH:44]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=3)[N:8]=2)[CH2:9]1)=[O:7])([CH3:3])([CH3:2])[CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 517165Ammonium AcetateHCID 67158091(RS)-4-{1-[5-(4-Fluorophenyl)-2-methylthiazol-4-yl]-methanoyl}-3-[2-(4-fluoro-phenyl)-2-oxo-ethoxycarbonylmethyl]-piperazine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 178433035HCID 178433035、化合物

実験手順

(RS)-4-{1-[5-(4-Fluorophenyl)-2-methylthiazol-4-yl]-methanoyl}-3-[2-(4-fluoro-phenyl)-2-oxo-ethoxycarbonylmethyl]-piperazine-1-carboxylic acid tert-butyl ester from description 111 (0.360 g) and anhydrous ammonium acetate were heated to 140° C. under argon for 1.5 hours with stirring. After cooling, the reaction mixture was partitioned between dichloromethane and saturated potassium carbonate solution. The organic solution was washed with brine, dried (MgSO4) and evaporated. The residue was chromatographed over silica gel, eluting with 0 to 10% ethanol in ethyl acetate. The title compound was obtained as a white foam (0.125 g), mass spectrum (API+) 580 [MH+], C30H31F2N5O3S requires 579.

後処理

  1. temperatureAfter cooling
  2. customthe reaction mixture was partitioned between dichloromethane and saturated potassium carbonate solution
  3. washThe organic solution was washed with brine
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customThe residue was chromatographed over silica gel
  7. washeluting with 0 to 10% ethanol in ethyl acetate

出典と根拠

ORDレコード
ord-2e6c52e290054983b1fe7e6833fab496
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07943645B2

反応ノート

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