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Sodium Sulfite → tert-Butyl 6-benzyloxy-3-{5-[3-(2,2-dimethylpropyl)cyclobutyl]-4-iodoisoxazole-3-yl}hexanoate

HRID 1912076
ノート
印刷プレビュー

反応式

HRID 1912076 の反応式
[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][CH:12]([C:21](=[N:33][O:34]C)[C:22]#[C:23][CH:24]1[CH2:27][CH:26]([CH2:28][C:29]([CH3:32])([CH3:31])[CH3:30])[CH2:25]1)[CH2:13][C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[I:36]Cl.S([O-])([O-])=O.[Na+].[Na+]>C(Cl)Cl>[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][CH:12]([C:21]1[C:22]([I:36])=[C:23]([CH:24]2[CH2:27][CH:26]([CH2:28][C:29]([CH3:32])([CH3:31])[CH3:30])[CH2:25]2)[O:34][N:33]=1)[CH2:13][C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24437Sodium SulfiteHCID 24640Iodine chlorideHCID 86675044tert-Butyl 3-(3-benzyloxypropyl)-6-[3-(2,2-dimethylpropyl)cyclobutyl]-4-methoxyimino-5-hexynoate

生成物 1

HCID 71127330tert-Butyl 6-benzyloxy-3-{5-[3-(2,2-dimethylpropyl)cyclobutyl]-4-iodoisoxazole-3-yl}hexanoate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

tert-Butyl 3-(3-benzyloxypropyl)-6-[3-(2,2-dimethylpropyl)cyclobutyl]-4-methoxyimino-5-hexynoate (3.37 g) and methylene chloride (70 mL) were mixed. To the mixture was added iodine monochloride (1 M in methylene chloride) (7.66 mL) at ice temperature. The mixture was stirred at ice temperature for 1 hr, and then to the mixture was added aqueous solution of sodium sulfite. The mixture was extracted with chloroform. The organic layer was washed with water and brine, then dried over magnesium sulfate. The magnesium sulfate was filtered off and the filtrate was concentrated in vacuo to give the title compound (4.21 g) as a crude product.

後処理

  1. extractionThe mixture was extracted with chloroform
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationThe magnesium sulfate was filtered off
  5. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-31367f32e21449c5bb87bc5353003ff5
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08604069B2

反応ノート

読み込み中…

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