p-Toluenesulfonic acid → HCID 19937311、化合物

HRID 36589ノート

反応式

HRID 36589 の反応式
[F:1][C:2]([F:23])([CH2:11][N:12]1[C:16](=[O:17])[C:15]2=[CH:18][CH:19]=[CH:20][CH:21]=[C:14]2[C:13]1=[O:22])[CH2:3][O:4]C1CCCCO1.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(O)C>[F:23][C:2]([F:1])([CH2:11][N:12]1[C:16](=[O:17])[C:15]2=[CH:18][CH:19]=[CH:20][CH:21]=[C:14]2[C:13]1=[O:22])[CH2:3][OH:4]

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 19937334HCID 19937334、化合物

生成物 1

HCID 19937311HCID 19937311、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2,2-difluoro-3-phthalimido-1-tetrahydropyranyloxypropane (2 g, 6.15 mmol), paratoluene sulfonic acid (0.1 g) in absolute ethanol was stirred overnight at room temperature. Then the mixture was concentrated in vacuo, diluted with ethyl acetate and .,washed with brine. The organic phase was separated, dried over magnesium sulfate and concentrated in vacuo. The crude alcohol 2,2-difluoro-3-phthalimido-1-propanol (1.4 g) was used for the next step without further purification.

後処理

  1. concentrationThen the mixture was concentrated in vacuo
  2. additiondiluted with ethyl acetate
  3. customThe organic phase was separated
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe crude alcohol 2,2-difluoro-3-phthalimido-1-propanol (1.4 g) was used for the next step without further purification

出典と根拠

ORDレコード
ord-6e5d03d2f4b843e893a93aa80a544745
出典データセット
uspto-grants-1995_05
特許番号
US05416076

反応ノート

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