Sodium Hydroxide → HCID 178505473, 화합물

HRID 728640

반응식

HRID 728640 반응식
[F:1][C:2]1[CH:11]=[CH:10][C:5]2[NH:6][C:7]([SH:9])=[N:8][C:4]=2[CH:3]=1.Cl.[CH:13]1([CH2:16][O:17][C:18]2[CH:23]=[CH:22][N:21]=[C:20]([CH2:24]Cl)[CH:19]=2)[CH2:15][CH2:14]1.[OH-].[Na+]>O.CO>[F:1][C:2]1[CH:11]=[CH:10][C:5]2[NH:6][C:7]([S:9][CH2:24][C:20]3[CH:19]=[C:18]([O:17][CH2:16][CH:13]4[CH2:15][CH2:14]4)[CH:23]=[CH:22][N:21]=3)=[N:8][C:4]=2[CH:3]=1

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 193909394-Cyclopropylmethoxy-2-chloromethylpyridine hydrochlorideHCID 178505474HCID 178505474, 화합물

생성물 1

HCID 178505473HCID 178505473, 화합물수율 82.5%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 962Water용매2회

실험 절차

To 5-fluoro-2-mercapto-1H-benzimidazole (0.88 g, 0.0051 mol) in methanol (25 ml) NaOH (0.2 g, 0.0051 mol) dissolved in H2O (1 ml) and 4-cyclopropylmethoxy-2-chloromethylpyridine hydrochloride (0.91 g, 0.0046 mol) dissolved in methanol (10 ml) were added in the given order. The mixture was heated to boiling and NaOH (0.2 g, 0.005 mol) dissolved in H2O (1 ml) was added and the mixture was refluxed for 1 hour. After evaporation of methanol, CH2Cl2 (75 ml) and H2O (50 ml) were added and pH adjusted to 10. The mixture was vigorously stirred, the phases were separated, the organic phase was dried over Na2SO4 and evaporated giving the desired product (1.25 g, 72%). NMR data for the product is given below.

후처리

  1. additionwere added in the given order
  2. additionwas added
  3. temperaturethe mixture was refluxed for 1 hour
  4. customAfter evaporation of methanol, CH2Cl2 (75 ml) and H2O (50 ml)
  5. additionwere added
  6. customthe phases were separated
  7. dry with materialthe organic phase was dried over Na2SO4
  8. customevaporated

출처 및 근거

ORD 기록
ord-619cf0d7650044b68aaca58664d6dd1e
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05049674

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