Tetrahydrofuran → HCID 67774375, 화합물

HRID 1963080노트

반응식

HRID 1963080 반응식
[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[N:10][N:9]2[C:12]([CH:30]=[O:31])=[C:13]([CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([F:28])[C:23]=3[CH3:29])[C:14]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[C:8]2[C:7]=1[Cl:32])=[O:5])[CH3:2].C=C(C)C.C1C[O:40]CC1.P([O-])(O)(O)=O.[Na+].Cl([O-])=O.[Na+]>C(O)(C)(C)C.O.[Cl-].[Na+].O.C(Cl)Cl.CC(=O)OCC>[Cl:32][C:7]1[C:8]2[N:9]([C:12]([C:30]([OH:40])=[O:31])=[C:13]([CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([F:28])[C:23]=3[CH3:29])[C:14]=2[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:10]=[CH:11][C:6]=1[C:4]([O:3][CH2:1][CH3:2])=[O:5]

참가 물질

11

반응물 5

HCID 8028TetrahydrofuranHCID 8255IsobutyleneHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphateHCID 88415083HCID 88415083, 화합물

생성물 1

HCID 67774375HCID 67774375, 화합물수율 98.1%

시약·촉매·용매 5

HCID 962Water용매2회HCID 6344Dichloromethane용매HCID 6386tert-Butanol용매HCID 8857Ethyl Acetate용매HCID 57417360Sodium chloride; water용매

실험 절차

The compound of step 7 (5.15 g, 11.42 mmol) was suspended in tert-butanol (90 ml), and a 2 M solution of isobutene in THF (34.27 ml, 68.53 mmol), a solution of sodium dihydrogenphosphate (4.111 g, 34.27 mmol) in 25 ml of water and sodium chlorite (1.937 g, 17.13 mmol) were added. The mixture was stirred at room temperature for 2 h. Then brine (200 ml), water (50 ml), EA (400 ml) and DCM (100 ml) were added and the organic phase was separated, dried over magnesium sulfate, filtered and evaporated to dryness. The obtained solid was triturated several times with cyclohexane and dried in vacuo at 50° C. 5.23 g of the title compound were obtained as a yellow solid melting at 193-194° C.

후처리

  1. customthe organic phase was separated
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. customevaporated to dryness
  5. customThe obtained solid was triturated several times with cyclohexane
  6. customdried in vacuo at 50° C

출처 및 근거

ORD 기록
ord-cb9884dede1c403091f0651d580a27b1
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08415336B2

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