Water → HCID 66808527, 화합물

HRID 607319노트

반응식

HRID 607319 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 66808527HCID 66808527, 화합물수율 99%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-155cfaa2dd0145b6acad01c68b536902
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915411B2

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