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Hydrochloric Acid → HCID 22909006, 화합물

HRID 1378989
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HRID 1378989 반응식
C[O:2][C:3]([C:5]1[CH:28]=[CH:27][C:8](/[CH:9]=[CH:10]/[C:11]2[N:19]([CH3:20])[C:18]3[C:17](=[O:21])[N:16]([CH2:22][CH3:23])[C:15](=[O:24])[N:14]([CH2:25][CH3:26])[C:13]=3[N:12]=2)=[C:7]([O:29][CH3:30])[CH:6]=1)=[O:4].O1CCCC1.O.[OH-].[Li+].Cl>O.C(O)C>[CH2:22]([N:16]1[C:17](=[O:21])[C:18]2[N:19]([CH3:20])[C:11](/[CH:10]=[CH:9]/[C:8]3[CH:27]=[CH:28][C:5]([C:3]([OH:4])=[O:2])=[CH:6][C:7]=3[O:29][CH3:30])=[N:12][C:13]=2[N:14]([CH2:25][CH3:26])[C:15]1=[O:24])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 70046683HCID 70046683, 화합물

생성물 1

HCID 22909006HCID 22909006, 화합물수율 24%

시약·촉매·용매 2

HCID 702Ethanol용매
HCID 962
Water
용매

실험 절차

Compound 20 (108 mg, 0.262 mmol) obtained in Example 19 was suspended in a solvent mixture of 2 ml of tetrahydrofuran, 2 ml of ethanol, and 1 ml of water. To the suspension was added 55 mg (1.311 mmol) of lithium hydroxide monohydrate, and the resulting mixture was stirred at room temperature for 12 hours. The reaction mixture was acidified with 2N HCl, and the precipitated crystals were collected by filtration. The obtained crude crystals were purified by column chromatography (eluent: chloroform/methanol/acetic acid=40/1/1) to give 25 mg (yield 24%) of Compound 22, which was further recrystallized from isopropanol to give a yellow powder.

후처리

  1. filtrationthe precipitated crystals were collected by filtration
  2. customThe obtained crude crystals
  3. customwere purified by column chromatography (eluent: chloroform/methanol/acetic acid=40/1/1)

출처 및 근거

ORD 기록
ord-d7a9405e03f7434db2cd53eff0932f50
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05670498

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