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Hydrochloric Acid → HCID 178419031, 화합물

HRID 6853
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HRID 6853 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([NH2:15])[CH:12]=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:16]#[C:17][NH2:18].Cl.[OH-].[Na+]>O1CCOCC1>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([NH:15][C:17]([NH2:18])=[NH:16])[CH:12]=[CH:13][CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 9864CyanamideHCID 14798Sodium HydroxideHCID 928923-Benzyloxyaniline

생성물 1

HCID 178419031HCID 178419031, 화합물수율 98.4%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

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온도
80 °C

실험 절차

To a suspension of 3-benzyloxyphenylamine (20.0 g, 100.35 mmol) in 1,4-dioxane (150 mL) was added cyanamide (7.39 g, 175.95 mmol followed by 4M HCl in 1,4-dioxane (44 ml, 176.00 mmol). The resulting suspension was heated at 80° C. overnight then cooled to ambient temperature and 6N NaOH (35 ml, 210.00 mmol) was added. The volume of solution was reduced to 50 ml in vacuo and the resulting precipitate was collected by filtration. The solid product was dried under vacuum overnight to afford 23.8 g in 98.4% yield. 1H NMR (MeOH-d4) δ 6.4–7.5 (m, 9H), 5.1 (s, 2H).

후처리

  1. temperaturethen cooled to ambient temperature
  2. filtrationthe resulting precipitate was collected by filtration
  3. customThe solid product was dried under vacuum overnight
  4. customto afford 23.8 g in 98.4% yield

출처 및 근거

ORD 기록
ord-e6b1f13036c244b682cb1d3247b19d66
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07084159B2

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