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Methyl morpholine oxide → Methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate

HRID 322054
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HRID 322054 반응식
[Cl:1][C:2]1[C:11]([CH2:12]Br)=[C:10]([S:14]([CH3:17])(=[O:16])=[O:15])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].C[N+]1([O-])CC[O:22]CC1>C(#N)C>[Cl:1][C:2]1[C:11]([CH:12]=[O:22])=[C:10]([S:14]([CH3:17])(=[O:16])=[O:15])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 82029Methyl morpholine oxideHCID 10969914Methyl 3-bromomethyl-2-chloro-4-methylsulfonylbenzoate

생성물 1

HCID 18517410Methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

89.2 g (0.26 mol) of methyl 2-chloro-3-bromomethyl-4-methylsulfonylbenzoate are dissolved in 500 ml of acetonitrile and treated at room temperature with 52.0 g (0.444 mol) of N-methylmorpholine N-oxide. The batch is stirred at room temperature for 18 hours, concentrated in a rotary evaporator, taken up in dichloromethane and washed several times with water. After concentration in the rotary evaporator, 57.3 g (80% of theory) of methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate having a melting point of 104-105° C. are obtained.

후처리

  1. concentrationconcentrated in a rotary evaporator
  2. washwashed several times with water
  3. concentrationAfter concentration
  4. customin the rotary evaporator, 57.3 g (80% of theory) of methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate having a melting point of 104-105° C.
  5. customare obtained

출처 및 근거

ORD 기록
ord-b7736fdfbd1f45c49c562e8a5c558e06
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06211216B1

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