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Dimethylformamide → Trichloroacetonitrile

HRID 363352
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HRID 363352 반응식
[Cl:1][C:2]([Cl:27])([Cl:26])[C:3](=[NH:25])[O:4][C@H:5]1[O:22][C@H:21]([CH2:23][Cl:24])[C@@H:16]([O:17][C:18](=[O:20])[CH3:19])[C@H:11]([O:12][C:13](=[O:15])[CH3:14])[C@H:6]1[O:7][C:8](=[O:10])[CH3:9].[C:28](O)(=O)[CH3:29].[NH2:32]N.C[N:35]([CH3:38])C=O>>[Cl:1][C:2]([Cl:27])([Cl:26])[C:3]#[N:25].[N:32]12[CH2:29][CH2:28][CH2:38][N:35]=[C:5]1[CH2:6][CH2:11][CH2:16][CH2:21][CH2:23]2.[Cl:27][C:2]([Cl:1])([Cl:26])[C:3](=[NH:25])[O:4][C@H:5]1[O:22][C@H:21]([CH2:23][Cl:24])[C@@H:16]([O:17][C:18](=[O:20])[CH3:19])[C@H:11]([O:12][C:13](=[O:15])[CH3:14])[C@H:6]1[O:7][C:8](=[O:10])[CH3:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6228DimethylformamideHCID 165591Hydrazine, acetate (1:1)HCID 53638677O-(2,3,4-tri-O-acetyl-6-chloro-6-deoxy-alpha-D-glucopyranosyl) trichloroacetimidate

생성물 3

HCID 11011TrichloroacetonitrileHCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene
HCID 53638677
O-(2,3,4-tri-O-acetyl-6-chloro-6-deoxy-alpha-D-glucopyranosyl) trichloroacetimidate

실험 절차

Compound 54 is then converted in two steps into O-(2,3,4-tri-O-acetyl-6-chloro-6-deoxy-α-D-glucopyranosyl) trichloroacetimidate (55). First, the anomeric acetate group of compound 54 is selectively removed by reaction with hydrazine acetate. Preferably, this reaction is conducted by contacting compound 54 with from about 1.1 to about 1.5 equivalents of hydrazine acetate (prepared by known procedures from hydrazine and acetic anhydride) at a temperature of from about 0° C. to about 20° C. for about 5 to about 10 hours. Typically, the reaction is conducted in an anhydrous solvent, such as dimethylformamide. Treatment of the resulting product with trichloroacetonitrile in the presence of an amine, such as 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), provides compound 55. This reaction is typically conducted in an anhydrous inert organic solvent, such as dichloromethane, using an excess of trichloroacetonitrile.

후처리

  1. customFirst, the anomeric acetate group of compound 54 is selectively removed by reaction with hydrazine acetate
  2. customof from about 0° C. to about 20° C.
  3. customfor about 5 to about 10 hours

출처 및 근거

ORD 기록
ord-9accb4b529d04b4a999433ecfc09608c
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05874411

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