Water → Ethyl (3-chloro-4-{1,3-dioxo-4,9-bis[(phenylmethyl)oxy]-1,3-dihydro-2H-benzo[f]isoindol-2-yl}phenyl)acetate

HRID 913165ノート

反応式

HRID 913165 の反応式
[C:1]1([CH2:7][O:8][C:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[C:12]([O:19][CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[C:11]([C:27](O)=[O:28])[C:10]=2[C:30](O)=[O:31])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH2:33][C:34]1[CH:39]=[CH:38][C:37]([CH2:40][C:41]([O:43][CH2:44][CH3:45])=[O:42])=[CH:36][C:35]=1[Cl:46].O>CN(C1C=CN=CC=1)C.C(O)(=O)C>[Cl:46][C:35]1[CH:36]=[C:37]([CH2:40][C:41]([O:43][CH2:44][CH3:45])=[O:42])[CH:38]=[CH:39][C:34]=1[N:33]1[C:27](=[O:28])[C:11]2[C:12]([O:19][CH2:20][C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)=[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:18]3=[C:9]([O:8][CH2:7][C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[C:10]=2[C:30]1=[O:31]

参加物

6

反応物 3

HCID 962WaterHCID 4380201,4-Bis[(phenylmethyl)oxy]-2,3-naphthalenedicarboxylic acidHCID 17859298(4-Amino-3-chloro-phenyl)-acetic acid ethyl ester

生成物 1

HCID 58012507Ethyl (3-chloro-4-{1,3-dioxo-4,9-bis[(phenylmethyl)oxy]-1,3-dihydro-2H-benzo[f]isoindol-2-yl}phenyl)acetate

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 176Acetic Acid溶媒

実験手順

A mixture of 1 1,4-bis[(phenylmethyl)oxy]-2,3-naphthalenedicarboxylic acid (5.0 g, 11.68 mmol), ethyl (4-amino-3-chlorophenyl)acetate (4.74 g, 22.2 mmol) and DMAP (0.427 g, 3.59 mmol) were heated to 120° C. in acetic acid (20 ml) for 18 hours. Water was added and the mixture and resulting brown solid collected by filtration and washed with water. This was triturated with ether to give a cream solid which was collected by filtration and dried in the vacuum oven (5.34 g, 8.83 mmol). LC/MS: Rt=4.15, [MH]+ 606.

後処理

  1. customthe mixture and resulting brown solid
  2. filtrationcollected by filtration
  3. washwashed with water
  4. customThis was triturated with ether
  5. customto give a cream solid which
  6. filtrationwas collected by filtration
  7. customdried in the vacuum oven (5.34 g, 8.83 mmol)

出典と根拠

ORDレコード
ord-8fb15f0916914c888de841fe27f189db
出典データセット
uspto-grants-2011_09
特許番号
US08026270B2

反応ノート

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