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Triphenylphosphine → N-benzylaminosulfonamide

HRID 1735939
ノート
印刷プレビュー

反応式

HRID 1735939 の反応式
[S:1]([NH2:5])([NH2:4])(=[O:3])=[O:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH2:25]([CH:27]([CH2:31][CH2:32][CH2:33][CH3:34])[C:28]([O-])=O)C.[Na+]>C1C=CC=CC=1.C(OCC)(=O)C>[CH2:28]([NH:4][S:1]([NH2:5])(=[O:3])=[O:2])[C:27]1[CH:25]=[CH:34][CH:33]=[CH:32][CH:31]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11776TriphenylphosphineHCID 82267SulfamideHCID 23672331Sodium 2-ethylhexanoate

生成物 1

HCID 12354987N-benzylaminosulfonamide収率 64%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

The condensed sulfamide having an allyloxycarbonyl protecting group obtained as Sample No. 3 of Example 1 is dissolved in benzene (10 vol.), and triphenylphosphine (0.3 Eq.), sodium 2-ethylhexanoate (1.5 Eq.) in ethyl acetate, and palladium tetrakistriphenylphosphine (0.02 Eq.) are added thereto successively. The mixture is stirred at room temperature for 30 minutes. The reaction mixture is diluted with ethyl acetate, washed with water, dried, and concentrated in vacuo. The residue is recrystallized from toluene to give benzylsulfamide having the same physical constants as that obtained in Reference Example 1. Pale yellow crystals. Yield: 64%.

後処理

  1. customobtained as Sample No
  2. washwashed with water
  3. customdried
  4. concentrationconcentrated in vacuo
  5. customThe residue is recrystallized from toluene

出典と根拠

ORDレコード
ord-b9d9e9714487402284a77792be89d894
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05539102

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート