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Benzene → HCID 131728530、化合物

HRID 2425103
ノート
印刷プレビュー

反応式

HRID 2425103 の反応式
[Na].[BH4-].[Cl:3][CH2:4][C:5](O)=O.C1C=CC=CC=1.[CH3:14][O:15][C:16]([C:18]1[CH:19]=[C:20]([CH3:41])[C:21]2[O:27][C:26]3[C:28]([Cl:37])=[CH:29][C:30]([NH:32][CH2:33][CH2:34][CH2:35][Cl:36])=[CH:31][C:25]=3[CH2:24][S:23](=[O:39])(=[O:38])[C:22]=2[CH:40]=1)=[O:17]>C1COCC1>[CH3:14][O:15][C:16]([C:18]1[CH:19]=[C:20]([CH3:41])[C:21]2[O:27][C:26]3[C:28]([Cl:37])=[CH:29][C:30]([N:32]([CH2:5][CH2:4][Cl:3])[CH2:33][CH2:34][CH2:35][Cl:36])=[CH:31][C:25]=3[CH2:24][S:23](=[O:38])(=[O:39])[C:22]=2[CH:40]=1)=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 241BenzeneHCID 300Chloroacetic AcidHCID 131720715CID 131720715HCID 1317285294-Chloro-2-(3-chloropropylamino)-6-methyl-10,10dioxo-10,11-dihydro-5-oxa-10lambda*6*-thia-dibenzo[a,d]-cycloheptene-8-carboxylic acid methyl ester

生成物 1

HCID 131728530HCID 131728530、化合物

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

Powdered sodium-borohydride (0.33 g, 8.6 mmol) was added in portions at 0° C., to a solution of chloroacetic acid (1.68 g, 17 mmol) in THF (6 mL), and benzene (90 mL). Reaction mixture was warmed to room temperature and stirred for 1 h, and compound of Example 29a (1.3 g, 2.9 mmol) was added. Reaction mixture was refluxed for 3 h. Reaction mixture was cooled and quenched using sodium bicarbonate solution, and extracted with ethylacetate. Organic layer was washed with water (100 mL) and brine (50 mL). The crude product obtained was purified by column chromatography (silica gel, ethylacetate/pet-ether) to obtain the title compound. Yield: 1.25 g (87%); 1H NMR (DMSO-d6, 300 MHz): δ 2.00 (t, 2H, CH2), 2.63 (s, 3H, CH3), 3.66 (t, 2H, CH2), 3.69-3.80 (m, 6H, 3×CH2), 3.85 (s, 3H, OCH3), 5.16 (s, 2H, CH2), 6.74 (s, 1H, Ar), 6.85 (s, 1H, Ar), 8.08 (s, 1H, Ar), 8.14 (s, 1H, Ar); MS: m/e (EI) 506 (M+).

後処理

  1. customReaction mixture
  2. customReaction mixture
  3. temperaturewas refluxed for 3 h
  4. customReaction mixture
  5. temperaturewas cooled
  6. customquenched
  7. extractionextracted with ethylacetate
  8. washOrganic layer was washed with water (100 mL) and brine (50 mL)
  9. customThe crude product obtained
  10. customwas purified by column chromatography (silica gel, ethylacetate/pet-ether)

出典と根拠

ORDレコード
ord-db29b3a573b64a52a64f740070f84885
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07964631B2

反応ノート

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