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Sulfuric Acid → HCID 19922080, 화합물

HRID 327981
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HRID 327981 반응식
C([O:3][C:4](=[O:45])[CH2:5][CH2:6][C:7]1[CH:12]=[C:11]([C:13]2[O:14][C:15](=[O:23])[C:16]3[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=3[CH:18]=2)[CH:10]=[CH:9][C:8]=1[O:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][O:30][C:31]1[CH:41]=[CH:40][C:34]2[C:35](=[O:39])[CH2:36][CH2:37][O:38][C:33]=2[C:32]=1[CH2:42][CH2:43][CH3:44])C.O.[OH-].[Li+].S(=O)(=O)(O)[OH:50]>C1COCC1.O>[C:15]([C:16]1[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=1[CH2:18][C:13]([C:11]1[CH:10]=[CH:9][C:8]([O:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][O:30][C:31]2[CH:41]=[CH:40][C:34]3[C:35](=[O:39])[CH2:36][CH2:37][O:38][C:33]=3[C:32]=2[CH2:42][CH2:43][CH3:44])=[C:7]([CH2:6][CH2:5][C:4]([OH:3])=[O:45])[CH:12]=1)=[O:50])([OH:14])=[O:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 1118Sulfuric AcidHCID 168937Lithium hydroxide, monohydrateHCID 53855288HCID 53855288, 화합물

생성물 1

HCID 19922080HCID 19922080, 화합물수율 79.6%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 0.145 g (0.24 mmol) of 2-[5-[(3,4-dihydro-4-oxo-8-propyl-2H-1-benzopyran-7-yl)oxy]pentyloxy]-5-(1-oxo-1H-2-benzopyran-3-yl)benzenepropanoic acid ethyl ester in 5 mL of THF and 5 mL of water was treated with 29.8 mg (0.71 mmol) of lithium hydroxide monohydrate and the mixture was stirred for 47 hrs. After being acidified with 16 mL of 3N aqueous sulfuric acid, the resulting mixture was worked up in the usual manner. The crude product was crystallized from hexane-ethyl acetate to give 0.114 g (79.6%) of the title compound as a white solid, mp 178°-182° C.

후처리

  1. customThe crude product was crystallized from hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-5e77ad63937d4fd2927d6fc549728ae3
출처 데이터셋
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05273999

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