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Acetic Acid → 2-(1-Benzyl-5-chloro-3-hydroxy-2-oxo-2,3-dihydro-1H-indol-3-yl)-N,N-dimethyl-acetamide

HRID 1991583
ノート
印刷プレビュー

反応式

HRID 1991583 の反応式
[CH2:1]([N:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([CH2:18][C:19]([N:21]([CH3:23])[CH3:22])=[O:20])([OH:17])[C:9]1=[O:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:25]N1C(=O)CCC1=O.C(O)(=O)C.C1(C)C=CC=CC=1>O>[CH2:1]([N:8]1[C:16]2[C:11](=[CH:12][C:13]([Cl:25])=[CH:14][CH:15]=2)[C:10]([CH2:18][C:19]([N:21]([CH3:23])[CH3:22])=[O:20])([OH:17])[C:9]1=[O:24])[C:2]1[CH:3]=[CH:4][CH:5]=[CH: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

6

反応物 4

HCID 176Acetic AcidHCID 1140TolueneHCID 31398ChlorosuccinimideHCID 104039792-(1-Benzyl-3-hydroxy-2-oxo-2,3-dihydro-1H-indol-3-yl)-N,N-dimethyl-acetamide

生成物 1

HCID 100213452-(1-Benzyl-5-chloro-3-hydroxy-2-oxo-2,3-dihydro-1H-indol-3-yl)-N,N-dimethyl-acetamide収率 88.2%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

A flask is charged with 2-(1-benzyl-3-hydroxy-2-oxo-2,3-dihydro-1H-indol-3-yl)-N,N-dimethyl-acetamide (Example 18) (10 g, 30.83 mmol), N-chloro succinimide (NCS) (4.12 g, 30.83 mmol), acetic acid (40 mL), and toluene (20 mL). The orange suspension is then stirred over night and becomes a homogeneous solution. After the addition of about 5 mL of water, the solvent is removed on the rotavapor. To the residue, water is added, and the product is extracted with chloroform. After drying and removal of solvent 11 g of crude product is obtained which after chromatography on silica (toluene:ethyl acetate 1:1) gives the title product (9.76 g, 88%) as yellow foam. 1H-NMR (CDCl3,300 MHz) δ 2.74, 3.08 (AB, 2H, 2J=16.3 Hz, CH2CONMe2); 4.85 (s, 2H, NCH2Ph); 6.32 (br s, 1H, OH); 6.58 (d, 1H, 3J=8.2 Hz, H-7); 7.10 (dd, 1H, 4J=2.0 Hz, H-6); 7.13-7.32 (m, 5H, Ph); 7.46 (d, 1H, H-4). 13C-NMR (CDCl3, 75 MHz) δ 35.77, 37.77 (N(CH3)2); 38.80 (CH2CONMe2); 44.27 (CH2Ph); 74.65 (C-3); 110.72 (C-7); 125.10 (C-4); 127.33 (Ph ortho-C); 127.90 (Ph para-C); 128.54 (C-5); 129.00 (Ph meta-C); 129.49 (C-6); 132.80 (C-9); 135.26 (C-15); 141.08 (C-8); 170.31 (C-11); 175.96 (C-2).

後処理

  1. customthe solvent is removed on the rotavapor
  2. additionTo the residue, water is added
  3. extractionthe product is extracted with chloroform
  4. customAfter drying
  5. customremoval of solvent 11 g of crude product
  6. customis obtained which after chromatography on silica (toluene:ethyl acetate 1:1)

出典と根拠

ORDレコード
ord-848ae4a469f6459d870fec13bf8dbd20
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07645886B2

反応ノート

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