Ammonium Chloride → (4-Phenylthiophen-2-yl)methanol

HRID 2286190ノート

反応式

HRID 2286190 の反応式
[C:1]1([C:7]2[CH:8]=[C:9]([CH:12]=[O:13])[S:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[BH4-].[Na+].[NH4+].[Cl-]>C(O)C>[C:1]1([C:7]2[CH:8]=[C:9]([CH2:12][OH:13])[S:10][CH:11]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 4311764Sodium borohydrideHCID 50094674-Phenylthiophene-2-carbaldehyde

生成物 1

HCID 12941349(4-Phenylthiophen-2-yl)methanol収率 96.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A stirred suspension of 4-phenyl-2-thiophenecarboxaldehyde (4.32 g) in absolute ethanol (85 ml) was cooled in an ice-bath and treated with NaBH4 (1.06 g). After 20 min. the mixture was allowed to attain ambient temperature when stirring was continued for 6h. Saturated aqueous NH4Cl (30 ml) was then carefully added to the vigorously stirred mixture, and the resulting suspension extracted with ER (2×200 ml). The combined extracts were dried (Na2SO4 /K2CO3), filtered and evaporated to give the title compound (4.2 g) as crystals, m.p. 112°-113°.

後処理

  1. temperaturewas cooled in an ice-bath
  2. customto attain ambient temperature
  3. waitwas continued for 6h
  4. extractionthe resulting suspension extracted with ER (2×200 ml)
  5. dry with materialThe combined extracts were dried (Na2SO4 /K2CO3)
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-f46f420f079f4a459b52e7d8a6d35d06
出典データセット
uspto-grants-1982_04
特許番号
US04327092

反応ノート

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