Hydrochloric Acid → HCID 12970145, 화합물

HRID 458008노트

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HRID 458008 반응식
CSC.B.[N+:5]([CH2:8][C:9]1([CH2:15][C:16]#[N:17])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)([O-:7])=[O:6].CO.Cl>C1(C)C=CC=CC=1.O1CCOCC1>[N+:5]([CH2:8][C:9]1([CH2:15][CH2:16][NH2:17])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)([O-:7])=[O:6]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 11275397HCID 11275397, 화합물HCID 12423031(Dimethyl sulfide)trihydroboron

생성물 1

HCID 12970145HCID 12970145, 화합물수율 56.1%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 312751,4-Dioxane용매

반응 조건

온도
60 °C

실험 절차

Borane methyl sulphide (2.0 M in toluene, 1.3 mL, 2.6 mmol) was added to compound 3 (0.4 g, 2.2 mmol) in toluene (10 mL) under nitrogen. After heating to 60° C. for 3 hours, the mixture was allowed to cool, and 15 mL methanol was added followed by 15 mL 4 M HCl in dioxane. After reflux for 1 hour, the mixture was evaporated to dryness. Crystallization from ethyl acetate gave the required product as colorless crystals (0.23 g, 47%); mp 170–173° C.

후처리

  1. temperatureto cool
  2. temperatureAfter reflux for 1 hour
  3. customthe mixture was evaporated to dryness
  4. customCrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-7d4163abaf1641c888d8c2184146b26d
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07189747B2

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