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Water → 2-(1-{[6-Chloro-2-(methoxymethyl)imidazo[2,1-b][1,3,4]thiadiazol-5-yl]methyl}-5-oxopyrrolidin-3-yl)ethyl 4-methylbenzenesulfonate

HRID 69563
ノート
印刷プレビュー

反応式

HRID 69563 の反応式
C([O:8][CH2:9][CH2:10][CH:11]1[CH2:15][N:14]([CH2:16][C:17]2[N:24]3[C:20]([S:21][C:22]([CH2:25][O:26][CH3:27])=[N:23]3)=[N:19][C:18]=2[Cl:28])[C:13](=[O:29])[CH2:12]1)C1C=CC=CC=1.[S:30](Cl)([C:33]1[CH:39]=[CH:38][C:36]([CH3:37])=[CH:35][CH:34]=1)(=[O:32])=[O:31].C(N(CC)CC)C.O>FC(F)(F)C(O)=O.CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH3:37][C:36]1[CH:38]=[CH:39][C:33]([S:30]([O:8][CH2:9][CH2:10][CH:11]2[CH2:12][C:13](=[O:29])[N:14]([CH2:16][C:17]3[N:24]4[C:20]([S:21][C:22]([CH2:25][O:26][CH3:27])=[N:23]4)=[N:19][C:18]=3[Cl:28])[CH2:15]2)(=[O:32])=[O:31])=[CH:34][CH:35]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 67116479HCID 67116479、化合物

生成物 1

HCID 866714522-(1-{[6-Chloro-2-(methoxymethyl)imidazo[2,1-b][1,3,4]thiadiazol-5-yl]methyl}-5-oxopyrrolidin-3-yl)ethyl 4-methylbenzenesulfonate収率 89%

試薬・触媒・溶媒 3

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6344Dichloromethane溶媒
HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
0 °C

実験手順

4-[2-(benzyloxy)ethyl]-1-{[6-chloro-2-(methoxymethyl)imidazo[2,1-b][1,3,4]thiadiazol-5-yl]methyl}pyrrolidin-2-one a37 (300 mg, 0.69 mmol, 1 eq) is heated at 60° C. for 3 hours in trifluoroacetic acid (3 ml). The crude 1-{[6-chloro-2-(methoxymethyl)imidazo[2,1-b][1,3,4]thiadiazol-5-yl]methyl}-4-(2-hydroxyethyl)pyrrolidin-2-one a38 is obtained after cooling and evaporation of the volatiles under reduced pressure. Dichloromethane (10 ml) is added to the residue, the mixture is cooled to 0° C., then tosyl chloride (158 mg, 0.828 mmol, 1.2 eq), triethyl amine (0.48 ml, 3.45 mmol, 5 eq) and 4-dimethylamino-pyridine (8 mg, 10 mol %,) are added at 0° C. The reaction is kept for 1 h at 0° C., then warmed up to room temperature and stirring is pursued for 2 days. After hydrolysis (H2O, 10 ml) and extraction with CH2Cl2 (4×10 ml), the cumulated organic layers are dried over MgSO4, filtered and evaporated under reduced pressure. The residue is purified by flash chromatography over silicagel (eluent: CH2Cl2/MeOH 97:3) to afford 308 mg of 2-(1-{[6-chloro-2-(methoxymethyl)imidazo[2,1-b][1,3,4]thiadiazol-5-yl]methyl}-5-oxopyrrolidin-3-yl)ethyl 4-methylbenzenesulfonate a39.

後処理

  1. customThe crude 1-{[6-chloro-2-(methoxymethyl)imidazo[2,1-b][1,3,4]thiadiazol-5-yl]methyl}-4-(2-hydroxyethyl)pyrrolidin-2-one a38 is obtained
  2. temperatureafter cooling
  3. customevaporation of the volatiles under reduced pressure
  4. additionDichloromethane (10 ml) is added to the residue
  5. temperaturewarmed up to room temperature
  6. waitis pursued for 2 days
  7. dry with materialthe cumulated organic layers are dried over MgSO4
  8. filtrationfiltered
  9. customevaporated under reduced pressure
  10. customThe residue is purified by flash chromatography over silicagel (eluent: CH2Cl2/MeOH 97:3)

出典と根拠

ORDレコード
ord-09925e9978a241578ee4a82da8e9086c
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822508B2

反応ノート

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