Water → HCID 66808527、化合物

HRID 607319ノート

反応式

HRID 607319 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)=[C:4]([N+:16]([O-])=O)[CH:3]=1.[Cl-].[NH4+].O1CCCC1.O>CO.[Fe]>[NH2:16][C:4]1[CH:3]=[C:2]([Br:1])[CH:7]=[CH:6][C:5]=1[S:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1

参加物

7

反応物 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 610314684-(4-Bromo-2-nitro-phenylsulfanyl)-phenol

生成物 1

HCID 66808527HCID 66808527、化合物収率 99%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 887Methanol溶媒

実験手順

A mixture of the product from Example 238A (0.302 g, 0.926 mmol), iron powder (0.208 g, 3.7 mmol, 4.0 eq) and ammonium chloride (0.059 g, 1.11 mmol, 1.2 eq) in a mixture of methanol (6 mL), tetrahydrofuran (6 mL), and water (2 mL) was heated under reflux for 5 hours and then cooled to room temperature. The reaction mixture was filtered through Celite and the filter pad was rinsed with methanol (25 mL). The filtrate was evaporated under reduced pressure to leave a brown glassy solid (0.27 g, 99%) that was utilized without further purification.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours
  3. filtrationThe reaction mixture was filtered through Celite
  4. washthe filter pad was rinsed with methanol (25 mL)
  5. customThe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-155cfaa2dd0145b6acad01c68b536902
出典データセット
uspto-grants-2011_03
特許番号
US07915411B2

反応ノート

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