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 913165노트

반응식

HRID 913165 반응식
[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]

참가 물질

6

반응물 3

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

생성물 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

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-8fb15f0916914c888de841fe27f189db
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026270B2

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