Hydrochloric Acid → (R)-N-(2-Chloro-3-nitro-4-iodophenyl)-2-hydroxy-2-methyl-3,3,3-trifluoropropanamide

HRID 2120370노트

반응식

HRID 2120370 반응식
Cl.[Cl:2][C:3]1[C:8]([N+:9]([O-:11])=[O:10])=[C:7]([I:12])[CH:6]=[CH:5][C:4]=1[NH:13][C:14](=[O:26])[C@:15]([O:21][Si](C)(C)C)([CH3:20])[C:16]([F:19])([F:18])[F:17]>CO>[Cl:2][C:3]1[C:8]([N+:9]([O-:11])=[O:10])=[C:7]([I:12])[CH:6]=[CH:5][C:4]=1[NH:13][C:14](=[O:26])[C@:15]([OH:21])([CH3:20])[C:16]([F:18])([F:19])[F:17]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 69824807(R)-N-(2-chloro-3-nitro-4-iodophenyl)-2-trimethylsilyloxy-2-methyl-3,3,3-trifluoropropanamide

생성물 1

HCID 69882875(R)-N-(2-Chloro-3-nitro-4-iodophenyl)-2-hydroxy-2-methyl-3,3,3-trifluoropropanamide수율 95.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2M Hydrochloric acid (2.5 ml) was added to a solution of (R)-N-(2-chloro-3-nitro-4-iodophenyl)-2-trimethylsilyloxy-2-methyl-3,3,3-trifluoropropanamide (Method 69) (1150 mg) in MeOH (25 ml) and the reaction mixture was stirred for 4 hours at ambient temperature. The volatile material was removed by evaporation and the residue was partitioned between EtOAc (150 ml) and water (75 ml). The organic phase was separated, washed with brine (75 ml) and dried. The volatile material was removed by evaporation to give the title compound (943 mg). NMR: 1.58 (s, 3H), 7.70 (d, 1H), 8.00 (d, 1H); m/z 437.

후처리

  1. customThe volatile material was removed by evaporation
  2. customthe residue was partitioned between EtOAc (150 ml) and water (75 ml)
  3. customThe organic phase was separated
  4. washwashed with brine (75 ml)
  5. customdried
  6. customThe volatile material was removed by evaporation

출처 및 근거

ORD 기록
ord-8d96ea256d0343199d7ffdf3bf6c278f
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06689909B1

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