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Hydrochloric Acid → HCID 57900151、化合物

HRID 84534
ノート
印刷プレビュー

反応式

HRID 84534 の反応式
Cl.ClC1C=CC=C[C:4]=1[N:9]1C=NN=[C:10]1C1SC2C3C=CC(N)=CC=3OCCC=2C=1.CCN(C(C)C)C(C)C.ClCC(Cl)=O.Cl[CH2:44][C:45]([NH:47][C:48]1[CH:49]=[CH:50][C:51]2[C:57]3[S:58][C:59]([C:61]4[N:65]([C:66]5[CH:71]=[CH:70][CH:69]=[CH:68][C:67]=5[Cl:72])[CH:64]=[N:63][N:62]=4)=[CH:60][C:56]=3[CH2:55][CH2:54][O:53][C:52]=2[CH:73]=1)=[O:46].Cl.N(C)C.CCN(CC)CC>C(Cl)Cl>[Cl:72][C:67]1[CH:68]=[CH:69][CH:70]=[CH:71][C:66]=1[N:65]1[CH:64]=[N:63][N:62]=[C:61]1[C:59]1[S:58][C:57]2[C:51]3[CH:50]=[CH:49][C:48]([NH:47][C:45](=[O:46])[CH2:44][N:9]([CH3:10])[CH3:4])=[CH:73][C:52]=3[O:53][CH2:54][CH2:55][C:56]=2[CH:60]=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

9

反応物 7

HCID 313Hydrochloric AcidHCID 674DimethylamineHCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 81531DiisopropylethylamineHCID 57900378HCID 57900378、化合物HCID 66899984HCID 66899984、化合物

生成物 1

HCID 57900151
HCID 57900151、化合物
収率 20%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution of 2-(4-(2-chlorophenyl)-4H-1,2,4-triazol-3-yl)-4,5-dihydrobenzo[b]thieno[2,3-d]oxepin-8-amine HCl salt (0.5 g, 1.16 mmol) in dried DCM (30 mL) was added DIPEA (0.61 mL, 3.48 mmol). The solution was stirred at 0° C. for 20 min and 2-chloro-acetyl chloride (0.2 g, 1.74 mmol) was added dropwise. The mixture was allowed to reach room temperature and stirred for a further 2 hours. The reaction solution was poured into ice water and extracted with EtOAc. The organics were combined, dried over Na2SO4 and evaporated in vacuum to afford the crude product (0.45 g, yield: 82%). 2-chloro-N-(2-(4-(2-chlorophenyl)-4H-1,2,4-triazol-3-yl)-4,5-dihydrobenzo[b]thieno[2,3-d]oxepin-8-yl)acetamide (0.2 g, 0.424 mmol) was mixed with HCl salt of NH(CH3)2 (0.172 g, 2.12 mmol) and NEt3 (0.3 mL, 2.12 mmol) in 15 mL of DCM. The solution was stirred at room temperature for 4 hours and quenched with ice water. Extraction with EtOAc and evaporation of the organics gave the crude product. It was purified by preparative TLC to afford 237 (40 mg, isolated yield: 20%). 1H NMR (DMSO-d6, 400 MHz): δ 9.81 (s, 1H), 8.81 (s, 1H), 7.79-7.38 (m, 7H), 6.55 (s, 1H), 4.16 (t, J=5.2 Hz, 2H), 3.02 (s, 3H), 2.96 (t, J=5.2 Hz, 2H), 2.21 (s, 6H). MS: (ESI+) 480.1

後処理

  1. customto reach room temperature
  2. stirringstirred for a further 2 hours
  3. extractionextracted with EtOAc
  4. dry with materialdried over Na2SO4
  5. customevaporated in vacuum
  6. customto afford the crude product (0.45 g, yield: 82%)
  7. stirringThe solution was stirred at room temperature for 4 hours
  8. customquenched with ice water
  9. extractionExtraction
  10. customwith EtOAc and evaporation of the
  11. customorganics gave the crude product
  12. customIt was purified by preparative TLC

出典と根拠

ORDレコード
ord-f0bc3d545ca1484980a222d6520b64e1
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846762B2

反応ノート

読み込み中…

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