Tetrahydrofuran → HCID 67774375、化合物

HRID 1963080ノート

反応式

HRID 1963080 の反応式
[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]

参加物

11

反応物 5

HCID 8028TetrahydrofuranHCID 8255IsobutyleneHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphateHCID 88415083HCID 88415083、化合物

生成物 1

HCID 67774375HCID 67774375、化合物収率 98.1%

試薬・触媒・溶媒 5

HCID 962Water溶媒2 回HCID 6344Dichloromethane溶媒HCID 6386tert-Butanol溶媒HCID 8857Ethyl Acetate溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cb9884dede1c403091f0651d580a27b1
出典データセット
uspto-grants-2013_04
特許番号
US08415336B2

反応ノート

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