Hydrochloric Acid → HCID 22467245、化合物

HRID 381324

反応式

HRID 381324 の反応式
[F-].C([N+](CC)(CC)CC)C.[O:11]1[C:15]2[CH:16]=[CH:17][C:18]([CH:20]([C:36]3[C:44]4[C:39](=[CH:40][C:41]([CH2:45][O:46][Si](C(C)C)(C(C)C)C(C)C)=[CH:42][CH:43]=4)[N:38]([CH3:57])[CH:37]=3)[C:21]([NH:23][S:24]([C:27]3[CH:32]=[CH:31][C:30]([CH3:33])=[CH:29][C:28]=3[CH2:34][CH3:35])(=[O:26])=[O:25])=[O:22])=[CH:19][C:14]=2[O:13][CH2:12]1.Cl>C(#N)C>[O:11]1[C:15]2[CH:16]=[CH:17][C:18]([CH:20]([C:36]3[C:44]4[C:39](=[CH:40][C:41]([CH2:45][OH:46])=[CH:42][CH:43]=4)[N:38]([CH3:57])[CH:37]=3)[C:21]([NH:23][S:24]([C:27]3[CH:32]=[CH:31][C:30]([CH3:33])=[CH:29][C:28]=3[CH2:34][CH3:35])(=[O:26])=[O:25])=[O:22])=[CH:19][C:14]=2[O:13][CH2:12]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 69582Ethanaminium, N,N,N-triethyl-, fluoride (1:1)HCID 22467246HCID 22467246、化合物

生成物 1

HCID 22467245HCID 22467245、化合物収率 84.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Tetraethylammonium fluoride (312 mg, 2.18 mmol) was added to a stirred solution of the compound of step (g) (380 mg, 0.55 mmol) in acetonitrile (6 ml) at room temperature under a nitrogen atmosphere. After 12 H the mixture was poured into 1M hydrochloric acid (50 ml) and extracted into ethyl acetate (2×50 ml). The organic fractions were combined, dried (MgSO4) and concentrated in vacuo to give a yellow foam. Flash column chromatography (eluting with 98% dichloromethane/2% methanol) gave the product as a white solid (242 mg).

後処理

  1. extractionextracted into ethyl acetate (2×50 ml)
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. customto give a yellow foam
  5. washFlash column chromatography (eluting with 98% dichloromethane/2% methanol)

出典と根拠

ORDレコード
ord-23cd5a78594f423b8c469eb4457657cd
出典データセット
uspto-grants-2001_10
特許番号
US06306852B1

関連ノート

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