Sodium Hydroxide → HCID 178505473、化合物

HRID 1085110

反応式

HRID 1085110 の反応式
[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

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 193909394-Cyclopropylmethoxy-2-chloromethylpyridine hydrochlorideHCID 178505474HCID 178505474、化合物

生成物 1

HCID 178505473HCID 178505473、化合物収率 82.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 962Water溶媒2 回

実験手順

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-chloromethyl-pyridine 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.

後処理

  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

出典と根拠

ORDレコード
ord-9e28c8a7815d48509ff00b7084a858d4
出典データセット
uspto-grants-1991_04
特許番号
US05008278

関連ノート

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