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Dimethylformamide → HCID 178509601、化合物

HRID 351101
ノート
印刷プレビュー

反応式

HRID 351101 の反応式
[Cl:1][C:2]1[CH:19]=[C:18]([CH2:20][C:21](=O)[C:22]2[CH:26]=[C:25]([C:27](=[O:32])C(Cl)(Cl)Cl)[NH:24][CH:23]=2)[CH:17]=[CH:16][C:3]=1[CH2:4][N:5]1C(=O)C2C(=CC=CC=2)C1=O.[Cl:34][C:35]1[CH:36]=[C:37](NCCO)[CH:38]=[CH:39][C:40]=1[F:41].[C:46]([CH:50]([N:54](C)C)N(C)C)(C)(C)C.[OH2:57].[NH2:58]N.C[N:61]([CH:63]=O)C>C1COCC1.C(O)C>[Cl:34][C:35]1[CH:36]=[C:37]([CH:50]([NH:54][C:27]([C:25]2[NH:24][CH:23]=[C:22]([C:21]3[C:20]([C:18]4[CH:17]=[CH:16][C:3]([CH2:4][NH2:5])=[C:2]([Cl:1])[CH:19]=4)=[CH:63][NH:61][N:58]=3)[CH:26]=2)=[O:32])[CH2:46][OH:57])[CH:38]=[CH:39][C:40]=1[F:41]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6228DimethylformamideHCID 24654Hydrazine hydrate (1:1)HCID 129886122-(2-Chloro-4-{2-oxo-2-[5-(2,2,2-trichloro-acetyl)-1H-pyrrol-3-yl-]-ethyl}-benzyl)-isoindole-1,3-dioneHCID 15731881Tert-butyl bis(dimethylamino)-methaneHCID 22349678N-2-hydroxyethyl-3-chloro-4-fluoroaniline

生成物 1

HCID 178509601
HCID 178509601、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of compound 10 (1.0 mmol) in DMF (5 mL) was added (S) 3-chloro-4-fluoro phenyl glycinol (1.2 mmol), then stirred for 15 h. The solvent was concentrated under vacuum. To the residue (1.0 mmol) in THF (1 mL) was added tert-butyl bis(dimethylamino)-methane (1 mL, 5 mmol). The mixture was stirred for 15 h at 50° C. and then concentrated under vacuum. To the residue (1 mmol) was added C2H5OH (5 mL) and hydrazine hydrate (1 mL, 20 mmol). The mixture was refluxed for 3 h and cooled to room temperature. The solvents were removed under vacuum and the crude products were purified from preparatory HPLC. This afforded the product 11 as a white solid. 1HNMR (CD3OD) 7.6 (s, 1H), 7.4 (s, 1H), 7.2–7.4 (m, 3H), 7.1–7.2 (m, 1H), 7.0 (t, 1H), 6.8 (d, 2H), 4.9 (t, 1H), 4.1 (s, 2H), 3.6 (dd, 2H).

後処理

  1. concentrationThe solvent was concentrated under vacuum
  2. stirringThe mixture was stirred for 15 h at 50° C.
  3. concentrationconcentrated under vacuum
  4. temperatureThe mixture was refluxed for 3 h
  5. customThe solvents were removed under vacuum
  6. customthe crude products were purified from preparatory HPLC

出典と根拠

ORDレコード
ord-7580c8bafbfc42b0b08504546fd27780
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07183307B2

反応ノート

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