Water → HCID 18401890, 화합물

HRID 1018660노트

반응식

HRID 1018660 반응식
[CH:1]1[C:6]2[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:5]=2[CH:4]=[CH:3][C:2]=1[OH:12].C([O-])([O-])=O.[Cs+].[Cs+].Br[CH2:20][CH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1.O>CN(C=O)C>[CH:21]1([CH2:20][O:12][C:2]2[CH:3]=[CH:4][C:5]3[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][C:6]=3[CH:1]=2)[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1

참가 물질

6

반응물 4

HCID 962WaterHCID 10796Cesium carbonateHCID 137636Cyclohexane, (bromomethyl)-HCID 108882365H-Benzocyclohepten-2-ol, 6,7,8,9-tetrahydro-

생성물 1

HCID 18401890HCID 18401890, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

To a mixture of 6,7,8,9-tetrahydro-5H-benzocyclohepten-2-ol (Helvetica Chimica Acta 1947, 1883.) (9.9 g, 61.0 mmol) and Cs2CO3 (26.3 g, 73.2 mmol) in DMF (100 ML) was added (bromomethyl)cyclohexane (10.2 mL, 73.2 mmol). The mixture was heated to 60° C. for 18 h, dumped into water and extracted with ethyl acetate. The combined extracts were washed with water, dried over magnesium sulfate and concentrated to a solid. The solid was recrystallized from ethanol (13.0 g, 83%). m.p. 62-63° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe combined extracts were washed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated to a solid
  5. customThe solid was recrystallized from ethanol (13.0 g, 83%)

출처 및 근거

ORD 기록
ord-75597b37e63141ccac0cacb19b604733
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06482852B2

반응 노트

불러오는 중…