p-Toluenesulfonic acid → HCID 19937311、化合物

HRID 1032919ノート

反応式

HRID 1032919 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. washwashed with brine
  4. customThe organic phase was separated
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. 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-7aa0e2122a08404f848052d063812b1d
出典データセット
uspto-grants-1994_05
特許番号
US05308837

反応ノート

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